CN114843433A - MXene conductive paper and preparation method of paper battery - Google Patents
MXene conductive paper and preparation method of paper battery Download PDFInfo
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- C01B32/90—Carbides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
Abstract
The invention discloses MXene conductive paper and a preparation method of a paper battery, and belongs to the technical field of conductive materials. MXene conductive paper is mainly prepared from nano-layered material MXene or MXene material doped with non-metal elements (N and/or S) or metal elements without adding any additiveTi prepared by additive or adhesive and having excellent conductivity and mechanical strength 3 C 2 T x Conductive paper. Such a self-contained, soft, tough electrode with high capacity and long lifetime is critical for the development of next generation lithium-sulfur (Li-S) batteries.
Description
Technical Field
The invention belongs to the field of conductive materials, and particularly relates to MXene conductive paper and a preparation method of a paper battery.
Background
Using mature paper technology, conductive paper is used as current collectors and electrodes, providing a low cost, lightweight, and efficient energy reserve concept. The paper battery is mainly formed by coating or printing ink made of nano materials by using fiber paper as a carrier to form a battery or a super capacitor. The paper battery can be cut and bent, is environment-friendly and low in cost, and relates to a plurality of electronic products in the application field.
Two-dimensional transition metal carbides and/or nitrides (MXenes) are receiving increasing attention due to their high electrical conductivity, abundant surface functionality and excellent dispersibility in various solvents, and show competitive advantages in energy storage and conversion applications. zhang group inAdv. Funct. Mater. A tough, electrically conductive S @ Ti made by a filter-evaporation process is reported 3 C 2 T x Paper, a strong conductive paper sheet, inherits Ti 3 C 2 T x The excellent electrical conductivity and mechanical properties of the nanoplatelets, as evidenced by the nearly constant electronic conductivity and the absence of any cracks under repeated bending and asperity conditions. Furthermore, the in-situ formed sulfate complex layer, which is uniformly coated on Ti to significantly suppress the lithium polysulfide shuttling effect in Li-S batteries 3 C 2 T x A thick protective film on the surface. This further demonstrates that MXene can play an important role in further immobilizing lithium polysulfide diffusion and preparing flexible electrodes in lithium sulfur batteries.
At present, two-dimensional materials are paid more and more attention in the research of paper batteries, but the technical scheme of most patent applications is only to simply mix nano materials and paper pulp together to prepare a paper motor, or to add electrode active materials or add some additives (additives and/or adhesives), and does not consider the influence of the mixing effect of the nano materials and the additives on the conductivity of the paper batteries, so that the conductivity of the electrodes is not obviously improved, and the advantages of the nano conductive materials cannot be exerted.
Disclosure of Invention
The first purpose of the invention is to provide MXene conductive paper, which can be used as a positive electrode of a paper battery and a negative electrode of the paper battery, and has the advantages of improving specific capacity, stabilizing battery performance, prolonging battery life and the like when being applied to the field of the paper battery.
The second purpose of the present invention is to provide an MXene paper battery, which has the advantages of high battery capacity, stable performance, long service life, etc.
A third object of the present invention is to provide applications of MXene conductive paper, which are very wide, including power sources for wearable devices, micro supercapacitors, metal ion batteries (including lithium, sodium, potassium, aluminum ion batteries), lithium sulfur batteries, etc., and the present invention is not limited to the applications thereof.
In order to achieve the first object of the present invention, the following technical solutions are adopted:
a flexible MXene conductive paper is mainly made of MXene materials without any additives including additives and/or adhesives.
Compared with the prior art, the MXene conductive paper provided by the invention mainly depends on the characteristics of MXene or improves MXene materials, including but not limited to N-doped Mxene, S-doped MXene, N and S Co-doped MXene, metal (Zn, Al, Cd, Fe, Co, Cu, Ni and Ag) doped MXene and one or more of MXene composite materials, so that the comprehensive conductive performance is improved. Under the condition of not adding an auxiliary agent, the MXene material has a good dispersing effect, and the flexible MXene conductive paper is prepared through suction filtration-evaporation. The MXene material has constant electronic conductivity, larger capacitance, stable charge and discharge performance, no crack under repeated bending and convex-concave conditions, and strong mechanical strength and chemical stability.
When the MXene conductive paper is used as a positive electrode paper or a negative electrode paper, any usable electrode material can be used for the other electrode.
MXene materials of the present invention include, but are not limited to, those comprising Sc 2 C、Sc 2 N、Ti 2 C、Ti 2 N、V 2 C、V 2 N、Cr 2 C、Cr 2 N、Zr 2 C、Zr 2 N、Nb 2 C、Nb 2 N、Hf 2 C、Hf 2 N、Ta 2 C、Mo 2 C、Ti 3 C 2 、Ti 3 N 2 、V 3 C 2 、Ta 3 C 2 、Ta 3 N 2 、Mo 3 C 2 、(Mo 4 V)C 4 、(Cr 2/3 Ti 1/2 ) 3 C 2 、 Ti 4 C 3 、Ti 4 N 3 、V 4 C 3 、V 4 N 3 、Ta 4 C 3 、Ta 4 N 3 、Nb 4 C 3 Or a combination thereof; n is doped with Mxene, S is doped with MXene, N and S are Co-doped with MXene, metal (Zn, Al, Cd, Fe, Co, Cu, Ni and Ag) is doped with MXene, and one or more of MXene composite materials are adopted; the preparation method comprises the steps of etching lithium fluoride and hydrochloric acid, etching HF, etching by a molten salt method and etching by a hydrothermal method assisted by NaOH; MXene material layer number monolayer, few layer even multilayer structure.
The MXene conductive paper can be prepared by a simple method which comprises the following steps: the MXene colloidal solution is directly filtered in vacuum through a polyethylene film and then naturally dried to prepare the MXene conductive paper.
In order to achieve the second object of the present invention, the following technical solutions are adopted:
the MXene paper battery relates to two types: one is to use the MXene conductive paper as the anode, the other is to use the MXene conductive paper as the cathode, and the two batteries have the advantages of excellent electronic conductivity, large electric capacity, stable charge and discharge performance, long battery life and the like.
When the positive electrode paper is mainly made of MXene conductive paper, the negative electrode paper is a metal foil with the potential lower than that of the positive electrode paper or a metal coating coated on the substrate; the metal foil or the metal coating is preferably metallic lithium or magnesium. Of course, the active material is not limited to these two types as long as a reversible charge and discharge function can be achieved.
When the positive electrode paper and the negative electrode paper are mainly made of MXene conductive paper, the positive electrode paper at least contains a positive electrode active material; the positive active material is mainly MXene material. Generally, the MXene paper battery is formed by sequentially laminating the positive electrode paper, the separator paper and the negative electrode paper, and the positive electrode paper, the separator paper and the negative electrode paper are immersed in an electrolyte and packaged. The separator paper may be made of any material as long as it has the function of separating the positive electrode and the negative electrode. The electrolyte is mainly selected according to the materials of the anode and the cathode, and the chemical reaction generated in the charge and discharge process is ensured to be reversible.
Compared with the prior art, the invention has the beneficial effects that:
(1) provided is MXene conductive paper having strong mechanical strength and chemical stability without any additive and without any crack in repeated bending and embossing;
(2) the MXene conductive paper has more uniform conductivity, no static problem, higher mechanical strength and chemical stability, and can improve the capacity and prolong the service life of the battery;
(3) the conductive paper and the paper battery can be widely applied to the application fields of power supplies of wearable devices, micro super capacitors, metal ion batteries (including lithium, sodium, potassium and aluminum ion batteries) and lithium-sulfur batteries, and a new way is opened up for the industrial application of the conductive paper and the paper battery.
Drawings
FIG. 1 is a schematic diagram of MXene conductive paper, which is (a) Ti 3 C 2 T x A conductive paper; (b) ti 2 CT x A conductive paper; (c) v 2 CT x Conductive paper.
FIG. 2 shows (a) Ti 2 CT x Conductive paper and (b) V 2 CT x XRD pattern of conductive paper.
FIG. 3 shows (a) Ti 3 C 2 T x SEM image of conductive paper and (b) Ti 3 C 2 T x Element distribution on the conductive paper.
Detailed Description
Reference will now be made in detail to the preferred embodiments of the present invention, but it will be understood by those skilled in the art that the following examples are illustrative only and should not be taken as limiting the scope of the present invention.
Example 1
Preparation of flexible MXene conductive paper and paper battery
1 g LiF was dissolved in 10 mL 6 MHCl and the solution was then mixed well. Then, 1 g of Ti was added over 30 minutes 3 AlC 2 The powder is gradually added to the mixed solution to avoid initial overheating. The reaction was stirred continuously at 35 ℃ for 24 hours. The obtained precipitate is washed and centrifuged alternately until the pH of the washing solution is greater than 6. The precipitate was vacuum filtered through a nylon membrane and then naturally dried, and then called multi-layer MXene (m-Ti) 3 C 2 T x ). To delaminate the nanoplatelets, 0.5g of m-Ti 3 C 2 T x The powder was dispersed in 150 mL of deionized water (DI-water). Sonicating for 1 h, and then centrifuging at 3500 rpm for 10 min to obtain a stable colloidal solution rich in a monolayer, but very little Ti 3 C 2 T x Nanosheets. Mixing Ti 3 C 2 T x The colloidal solution is directly filtered in vacuum through a polyethylene film and then naturally dried to prepare Ti 3 C 2 T x Paper. According to Ti 3 C 2 T x The positive electrode conductive paper, the diaphragm paper and the negative electrode paper are sequentially stacked or repeatedly stacked, and the positive electrode paper piece and the negative electrode paper piece are respectively connected to the current collectors and then packaged. After vacuumizing the reserved opening during packaging, injecting a proper amount of electrolyte, and finally sealing the reserved opening. And milling holes on the packaged paper battery, and connecting a current collector into a circuit to form the rechargeable paper sheet lithium battery.
Example 2
Preparation of flexible MXene conductive paper and paper battery
1 g LiF was dissolved in 10 mL 6 MHCl and the solution was then mixed well. Then, 1 g of Ti was added over 30 minutes 3 AlC 2 The powder is gradually added to the mixed solution to avoid initial overheating. The reaction was stirred continuously at 35 ℃ for 24 hours. The obtained precipitate is washed and centrifuged alternately until the pH of the washing solution is greater than 6. The precipitate was vacuum filtered through a nylon membrane and then naturally dried, and then called multilayer MXene (A), (B), (C) and D)m-Ti 3 C 2 T x ). The obtained m-Ti 3 C 2 T x 100mg of the powder is dispersed into 50ml of a lining of a hydrothermal kettle of 60 ℃ saturated urea solution, and the mixture is magnetically stirred for 3 hours at 60 ℃ to obtain uniform mixed solution. Then the hydrothermal reaction kettle is reacted for 12 hours at 180 ℃, deionized water is continuously used for washing until the pH value is about 7 after the reaction is finished, and then the reaction product is placed in a vacuum drying oven and dried for 12 hours at 60 ℃, and is marked as N-Ti 3 C 2 T x . For delamination of the nanoplatelets, 0.5g is noted as N-Ti 3 C 2 T x . The powder was dispersed in 150 mL of deionized water (DI-water). Ultrasonic treating for 1 h, centrifuging at 3500 rpm for 10 min to obtain stable colloidal solution rich in monolayer and very little layer of N-Ti 3 C 2 T x Nanosheets. Adding N-Ti 3 C 2 T x The colloidal solution is directly filtered in vacuum by a polyethylene film and then naturally dried to prepare N-Ti 3 C 2 T x Paper. For the prototype pouch half cell, the entire vacuum filtered N-Ti 3 C 2 T x Paper was used as the cathode and lithium tape as the anode. Aluminum and copper strips were connected to the sides of the two electrodes as connecting cables. All components are compactly stacked and enclosed in a self-sealing plastic bag.
Example 3
Preparation of flexible MXene conductive paper and paper battery
1 g LiF was dissolved in 10 mL 6 MHCl and the solution was then mixed well. Then, 1 g of Ti was added over 30 minutes 3 AlC 2 The powder is gradually added to the mixed solution to avoid initial overheating. The reaction was stirred continuously at 35 ℃ for 24 hours. The obtained precipitate is washed and centrifuged alternately until the pH of the washing solution is greater than 6. The precipitate was vacuum filtered through a nylon membrane and then naturally dried, and then called multi-layer MXene (m-Ti) 3 C 2 T x ). Firstly, the Ti is prepared 3 C 2 Grinding and mixing the powder and thiourea (the mass ratio is 1: 3) uniformly, then placing the mixture into a tube furnace under the Ar atmosphere, heating to 500 ℃, preserving heat for 3 hours, cooling to room temperature, grinding the prepared material again, and repeatedly washing the material by deionized water until the material is completely dissolvedAnd (4) the product is neutral. Drying the obtained powder to obtain the N, S co-doped Ti 3 C 2 Is denoted by N, S-Ti 3 C 2 T x . To delaminate the nanoplatelets, 0.5gN, S-Ti 3 C 2 T x Was dispersed in 150 mL of deionized water (DI-water). Ultrasonic treating for 1 h, centrifuging at 3500 rpm for 10 min to obtain stable colloidal solution rich in monolayer and very little layer of N, S-Ti 3 C 2 T x Nanosheets. Mixing N, S-Ti 3 C 2 T x Directly passing the colloidal solution through a polyethylene film for vacuum filtration, and naturally drying to prepare N, S-Ti 3 C 2 T x Paper. The prepared N, S-Ti 3 C 2 T x The paper is directly put into a disc with the mass of 2.5-3 mg, the diameter of 13 mm and the thickness of 7 mu m. For N, S-Ti 3 C 2 T x Paper/lithium half-cell, N, S-Ti 3 C 2 T x Paper was used as the working electrode, lithium foil counter/reference electrode, plus separator.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. The preparation method of MXene conductive paper and the paper battery is characterized by comprising the following steps:
(1) firstly, obtaining a nano monolayer MXene material from a MAX phase, and comprising the following methods:
i, etching MAX phase material by lithium fluoride and hydrochloric acid
Adding MAX phase materials into a mixed solution of lithium fluoride and hydrochloric acid, reacting, taking precipitates, washing and centrifuging the precipitates alternately until the pH value of a washing solution is more than 6, and drying to obtain a single-layer MXene material;
II, HF etching MAX phase material
Mixing the improved MAX phase raw material with HCl, deionized water and HF mixture, stirring overnight, centrifuging and washing to obtain multilayer sediment, then intercalating in LiCl solution, and repeatedly centrifuging and washing with deionized water to obtain a single-layer MXene material;
III, etching MAX phase material by molten salt method
Weighing improved MAX phase raw materials, chloride salt or bromide salt, NaCl and KCl, putting the obtained mixture into ball milling equipment, fully ball milling and uniformly mixing, then putting the ground powder into an alumina crucible, putting the alumina crucible into a tubular furnace, carrying out high-temperature reaction in an inert atmosphere, cooling, putting a reaction product into dilute hydrochloric acid for soaking, then carrying out ultrasonic cleaning, vibrating and standing, taking a precipitate, and repeatedly carrying out centrifugal cleaning and intercalation by using deionized water to obtain a single-layer MXene material;
IV NaOH-assisted hydrothermal etching of MAX phase materials
The MAX phase raw material is improved through NaOH treatment with a certain concentration, and MXene powder with the purity of 92 wt.% is prepared under the hydrothermal action;
(2) dispersing the obtained or improved nano layered MXene powder in deionized water, and performing ultrasonic dispersion to obtain a colloidal solution with a certain concentration;
(3) MXene conductive paper is obtained through different preparation processes and shape transformation.
2. The method of claim 1, wherein the MAX phase in step (1) comprises, but is not limited to, Ti 2 AlC、Ti 2 AlN、V 2 AlC、V 2 AlN、Nb 2 AlC、NbAl 2 N、Ta 2 AlC、Ti 3 AlC 2 、Ti 3 AlN 2 、V 3 AlC 2 、Ta 3 AlC 2 、Ta 3 AlN 2 、 Ti 4 AlC 3 、Ti 4 AlN 3 、Ta 4 AlC 3 、Ta 4 NAl 3 、Nb 4 AlC 3 One or more MAX phase ceramics, Mxene has a chemical formula of M n+1 X n T x Wherein M is at least one of groups 3, 4, 5, 6 or 7 of the periodic Table of the elements, wherein each X isC. N or a combination thereof N =1, 2, 3 or 4, T x For surface capping (radical), Mxene materials are included in the form of their representation M n+1 X n Containing Sc 2 C、Sc 2 N、Ti 2 C、Ti 2 N、V 2 C、V 2 N、Cr 2 C、Cr 2 N、Zr 2 C、Zr 2 N、Nb 2 C、Nb 2 N、Hf 2 C、Hf 2 N、Ta 2 C、Mo 2 C、Ti 3 C 2 、Ti 3 N 2 、V 3 C 2 、Ta 3 C 2 、Ta 3 N 2 、Mo 3 C 2 、(Mo 4 V)C 4 、(Cr 2/3 Ti 1/2 ) 3 C 2 、 Ti 4 C 3 、Ti 4 N 3 、V 4 C 3 、V 4 N 3 、Ta 4 C 3 、Ta 4 N 3 、Nb 4 C 3 Or a combination thereof; t is a unit of x Is a surface group comprising alkoxide, alkyl, carboxylate, halide, hydroxide, hydride, oxide, suboxide, nitride, subnitride, sulfide, sulfonate, thiol, or combinations thereof; the Mxene material has multiple layers, few layers or a single layer; the solvent in which the Mxene material is dissolved is water, alcohol, DMSO, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethyl ethylenediamine, acetone, triethylamine, n-butyl alcohol, dioxane, tetrahydrofuran, methyl formate, tributylamine, methyl ethyl ketone, ethyl acetate, chloroform, trioctylamine, dimethyl carbonate, diethyl ether, isopropyl ether, n-butyl ether, trichloroethylene, diphenyl ether, dichloromethane, dichloroethane, benzene, toluene, carbon tetrachloride, carbon disulfide, cyclohexane, hexane, petroleum ether.
3. The flexible MXene conductive paper and paper battery as claimed in claim 1, wherein the dispersion in step (2) includes but is not limited to stirring, ultrasound, crushing and other experimental processes; the improvement comprises but is not limited to one or more of N-doped Mxene, S-doped MXene, N, S-codoped MXene, metal (Zn, Al, Cd, Fe, Co, Cu, Ni, Ag) doped MXene, additives, adhesives and the like, and MXene composite materials.
4. The flexible MXene conductive paper and paper battery as claimed in claim 1, wherein the preparation process in step (3) includes but is not limited to vacuum filtration, pressing pipe and rolling film, manual grinding, spraying, 3D printing, silk screen printing, direct forming; topographical transformations include, but are not limited to, sheets, layers, wires, blocks, strips, plates of various shapes.
5. A flexible MXene conductive paper and a paper battery, wherein one of positive electrode paper or negative electrode paper of the MXene paper battery is mainly made of the MXene conductive paper of any one of claims 1-4.
6. The MXene paper battery of claim 5, wherein the positive electrode paper is mainly made of the MXene conductive paper, and the negative electrode paper is a metal foil with a potential lower than that of the positive electrode paper or a metal coating coated on a substrate; the metal foil or the metal coating is preferably metallic lithium or magnesium.
7. The MXene paper battery of claim 5, wherein the positive and negative electrode paper is mainly made of MXene conductive paper, and the positive electrode paper contains at least a positive electrode active material; the positive active material is mainly MXene material.
8. The MXene paper battery according to any one of claims 3-7, wherein the MXene paper battery is formed by laminating the positive electrode paper, separator paper and the negative electrode paper in this order, and the positive electrode paper, separator paper and the negative electrode paper are immersed in an electrolyte and packaged.
9. An MXene conductive paper according to any one of claims 1-5, wherein the MXene conductive paper is used for making power source including but not limited to wearable device, micro super capacitor, metal ion battery (including lithium, sodium, potassium, aluminum ion battery), lithium sulfur battery.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114835119A (en) * | 2022-06-10 | 2022-08-02 | 哈尔滨工业大学（深圳） | Single-layer Nb 2 CT x MXene and aluminum ion battery positive plate and preparation method thereof |
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Cited By (1)
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| CN114835119A (en) * | 2022-06-10 | 2022-08-02 | 哈尔滨工业大学（深圳） | Single-layer Nb 2 CT x MXene and aluminum ion battery positive plate and preparation method thereof |
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