CN114843510A - Preparation method of metal-sulfur in-situ co-doped MXene electrode material - Google Patents

Preparation method of metal-sulfur in-situ co-doped MXene electrode material Download PDF

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CN114843510A
CN114843510A CN202110131203.4A CN202110131203A CN114843510A CN 114843510 A CN114843510 A CN 114843510A CN 202110131203 A CN202110131203 A CN 202110131203A CN 114843510 A CN114843510 A CN 114843510A
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CN114843510B (en
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何青
胡慧慧
章冬雯
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Suzhou Beike Nano Technology Co ltd
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Abstract

The invention discloses a preparation method of a metal-sulfur in-situ co-doped MXene electrode material, and belongs to the technical field of conductive materials. A metal-sulfur in-situ co-doped MXene electrode material is prepared by firstly preparing sulfur-doped MAX phase ceramic, then performing element replacement on an A phase of S-MAX through a Lewis molten salt reaction to synthesize a metal-embedded nano layered MAX phase, and then preparing a two-dimensional layered nano material MXene by etching and removing an A metal atomic layer in the MAX phase material through a chemical etching method. The invention designs an independent, firm and durable electrode material with high capacity and long service life, which can effectively solve the great limitation of lithium polysulfide (LipS) shuttle effect and is very important for developing high-grade lithium-sulfur (Li-S) batteries for next-generation electronic equipment.

Description

Preparation method of metal-sulfur in-situ co-doped MXene electrode material
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to a preparation method of a metal-sulfur in-situ co-doped MXene electrode material.
Background
In order to meet the increasing demands of electric vehicles and power grid applications, high energy density rechargeable batteries, particularly lithium ion batteries, are widely used. However, lithium batteries have generated concern due to the high cost and availability of lithium resources. The room temperature sodium-sulfur battery and the lithium-sulfur battery have development prospects due to the advantages of high theoretical energy density, large sodium-lithium-sulfur storage capacity, low cost and the like. However, sodium-sulfur batteries and lithium-sulfur batteries have disadvantages of low reversible capacity, poor self-discharge and cycle performance, etc., which have prevented their wide application. The natural insulating properties of elemental sulfur limit its use as an active material, resulting in slow kinetics of the electrochemical process of the cathode. Meanwhile, the solubility of the reduced sodium polysulfide is more serious than that of the lithium polysulfide in the charging and discharging processes, so that the uncontrollable shuttling effect of the sodium polysulfide is aggravated, and the cycle life of the sodium-sulfur battery is poor. Due to the two-dimensional structure, the functional surface, the high conductivity and the chemical durability of the battery, MXenes has wide application prospects in the aspects of rechargeable batteries, supercapacitors, catalysts, electromagnetic shielding, electrochromic materials, antennas and the like. Particularly in the fields of high-rate lithium-sulfur batteries, capacitors, sodium batteries, and the like.
Sodium-sulfur batteries and lithium-sulfur batteries use abundant elements and provide an attractive alternative to the batteries currently in use, but they require better sulfur-containing materials to compete with lithium-ion batteries for capacity and cycling capability. The invention provides an in-situ sulfur doping strategy, which is characterized in that MXene nano-flake is functionalized by introducing heteroatom sulfur from a MAX precursor and a co-doped metal (M) into an MXene structure. A vacuum freeze-drying method is adopted to prepare the three-dimensional folded MXene nanostructure with high specific surface area. In a room-temperature sodium-sulfur battery and a lithium-sulfur battery, special shrinkage sulfur-doped MXene (M, S-MXene) nanosheets are adopted as electrode main materials. M, S-MXene is highly polar with sodium polysulfide and lithium polysulfide, limiting the diffusion of sodium polysulfide and lithium polysulfide.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a metal-sulfur in-situ co-doped MXene electrode material, which can be used as a positive electrode material and a negative electrode material, and has the advantages of improving specific capacity, stabilizing battery performance, prolonging battery life and the like when being applied to the field of batteries.
A second object of the present invention is to provide applications of MXene electrode material, which are very wide, including power sources for wearable devices, micro supercapacitors, metal ion batteries (including lithium, sodium, potassium, aluminum, zinc ion batteries), lithium sulfur batteries, sodium sulfur batteries, solid state batteries, semi-solid state 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:
the preparation method of the metal-sulfur in-situ co-doped MXene electrode material comprises the following specific steps:
firstly, titanium, aluminum, graphite and sulfur are mixed according to a certain atomic ratio to synthesize the MAX powder doped with polycrystalline sulfur. The powder mixture was sintered in a high temperature tube furnace in flowing argon. The MAX product produced was ground and sieved through a 200 mesh screen. Sulphur doped MAX phase powder was obtained.
To synthesize metal-sulfur in situ co-doped MXene, sulfur doped MAX is first mixed with lewis molten salt in a molar ratio. The raw materials were thoroughly mixed in a glove box with a mortar under nitrogen blanket. The resulting mixture powder was then taken out of the glove box and placed in an alumina crucible. The alumina crucible was loaded into a tube furnace and calcined under inert atmosphere. After the reaction, the product was washed with deionized water to remove residual molten salt, and the final product was dried. And finally, obtaining the metal-sulfur in-situ co-doped MXene material.
Preferably, the MAX phase 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 a combination of two or more MAX phase ceramics;
preferably, the MXene comprises 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;
preferably, the sintering tube is a quartz tube of a high-temperature tube furnace, and the calcining temperature can reach 1650 ℃;
preferably, the inert atmosphere is argon;
preferably, the sulfur doping is a mixture of titanium, aluminum, graphite and sulfur which are uniformly mixed according to different atomic ratios;
preferably, the sulphur-doped MAX phase powder is mixed with the lewis molten salt in a stoichiometric molar ratio of 1: 1-1: 10, mixing;
preferably, the MXene embedding metal comprises Ni, Co, Zn, Cd, Fe, Cu, Ag;
preferably, the reaction centrifugation is specifically centrifugation for 5-15 min at the speed of 3000-6000 rpm;
preferably, the reaction drying is vacuum drying for 6-24 hours at 30-80 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) during the manufacture of a cathode material for a lithium-sulfur battery, sulfur is incorporated into a cathode body, which itself has high electronic conductivity, excellent mechanical flexibility, and abundant chemical interaction sites. The in-situ formation of a protective barrier on a robust conductive cathode during cycling to immobilize polysulfide shuttling not only improves sulfur utilization, but also greatly simplifies the manufacturing process;
(2) the sulfur-doped MXene electrode material can effectively relieve poor cycle performance and low utilization rate of active materials of the lithium-sulfur battery, and polysulfide and volume expansion limit the use problems of the lithium-sulfur battery and the sodium-sulfur battery in practical application;
(3) the single-layer two-dimensional MXene material prepared by embedding metal atoms such as Ni, Co and the like has obviously enhanced electrochemical performance, can be applied to the electrochemical field, such as metal ion batteries (including lithium, sodium, potassium, aluminum and zinc ion batteries), lithium-sulfur batteries, solid-state batteries, semi-solid-state batteries and the like, and widens the application field of the MXene material.
Drawings
FIG. 1 shows metal particles uniformly dispersed in Ti 3 C 2 SEM image on top.
Fig. 2 is a physical diagram of different electrode materials, (a) metal-sulfur in-situ co-doped MXene ink and clay; (2) a flexible electrode material; (3) a nickel electrode material.
Detailed Description
The preferred embodiments of the present invention will be described in detail below.
Example 1
Preparation of metal-sulfur in-situ co-doped MXene electrode material
Firstly, mixing titanium, aluminum, graphite and sulfur in a certain atomic ratio to synthesize the MAX powder (Ti) doped with polycrystalline sulfur 3 AlC 2 S x ). The powder mixture was sintered in a high temperature tube furnace at 1650 ℃ under flowing argon. The heating rate was 5 ℃ per min. The MAX product produced was ground and sieved through a 200 mesh screen. Sulphur-doped MAX-phase powder (Ti) is obtained 3 AlC 2 S x ) (particle size)<74 μm). To synthesize the metallic embedded MAX phase, MAX is first combined with CoCl 2 MeltingSalt molar ratio 1: 6 mixing the powder as a starting material. The raw materials were thoroughly mixed in a glove box with a mortar under nitrogen blanket. The resulting mixture powder was then taken out of the glove box and placed in an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated at 700 ℃ for 24h under argon protection. After the reaction, the product was washed with deionized water to remove residual CoCl 2 And the final product was dried at 40 ℃. Finally, Co-S Co-doped MXene material (Co, S-Ti) is obtained 3 C 2 ）。
Example 2
Preparation of metal-sulfur in-situ co-doped MXene electrode material
Firstly, mixing titanium, aluminum, graphite and sulfur in a certain atomic ratio to synthesize the MAX powder (Ti) doped with polycrystalline sulfur 3 AlC 2 S x ). The powder mixture was sintered in a high temperature tube furnace at 1650 ℃ under flowing argon. The heating rate was 5 ℃ per min. The MAX product produced was ground and sieved through a 200 mesh screen. Sulphur-doped MAX-phase powder (Ti) is obtained 3 AlC 2 S x ) (particle size)<74 μm). To synthesize the metallic embedded MAX phase, MAX is first combined with NiCl 2 Molten salt molar ratio 1: 6 mixing the powder as a starting material. The raw materials were thoroughly mixed in a glove box with a mortar under nitrogen blanket. The resulting mixture powder was then taken out of the glove box and placed in an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated at 700 ℃ for 24h under argon protection. After the reaction, the product was washed with deionized water to remove residual NiCl 2 And the final product was dried at 40 ℃. Finally, Ni-S co-doped MXene material (Ni, S-Ti) is obtained 3 C 2 ）。
Example 3
Preparation of metal-sulfur in-situ co-doped MXene electrode material
Firstly, mixing titanium, aluminum, graphite and sulfur in a certain atomic ratio to synthesize the MAX powder (Ti) doped with polycrystalline sulfur 3 AlC 2 S x ). The powder mixture was sintered in a high temperature tube furnace at 1600 ℃ under flowing argon. The heating rate was 5 ℃ per min. Will make intoThe resulting MAX product was ground and sieved through a 200 mesh screen. Sulphur-doped MAX-phase powder (Ti) is obtained 3 AlC 2 S x ) (particle size)<74 μm). To synthesize the metallic embedded MAX phase, MAX is first combined with CoCl 2 、NiCl 2 Molten salt molar ratio 1: 3: 3 mixing the powders as starting materials. The raw materials were thoroughly mixed in a glove box with a mortar under nitrogen blanket. The resulting mixture powder was then taken out of the glove box and placed in an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated at 700 ℃ for 24h under argon protection. After the reaction, the product was washed with deionized water to remove residual CoCl 2 、NiCl 2 And the final product was dried at 40 ℃. Finally, Co, Ni and S Co-doped MXene material (Co, Ni, S-Ti) is obtained 3 C 2 ）。
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 (6)

1. A preparation method of a metal-sulfur in-situ co-doped MXene electrode material is characterized by comprising the following steps: firstly, mixing titanium, aluminum, graphite and sulfur according to a certain atomic ratio to synthesize polycrystal sulfur-doped MAX powder, sintering the powder mixture in a high-temperature tube furnace in flowing argon, grinding the prepared MAX product and sieving the MAX product by a 200-mesh sieve to obtain sulfur-doped MAX phase powder; in order to synthesize the metal-sulfur in-situ co-doped MXene, firstly mixing sulfur-doped MAX and Lewis molten salt according to a molar ratio, fully mixing the raw materials in a glove box by using a mortar under the protection of nitrogen, then taking the obtained mixture powder out of the glove box, putting the mixture powder into an alumina crucible, putting the alumina crucible into a tubular furnace, calcining the mixture powder under the protection of an inert atmosphere, washing the product with deionized water after reaction to remove residual molten salt, drying the final product, and finally obtaining the metal-sulfur in-situ co-doped MXene material.
2. The method for preparing the metal-sulfur in-situ co-doped MXene electrode material as claimed in claim 1, wherein the MAX phase comprises Ti and not limited thereto 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 is C, 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 x Is a surface group comprising alkoxide, alkyl, carboxylate, halide, hydroxide, hydride, oxide, sub-oxide, metal oxide, or metal oxide,A nitride, a nitridate, a sulfide, a sulfonate, a thiol, or a combination 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, acetonitrile, DMF, hexamethylphosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butanol, 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 method for preparing the metal-sulfur in-situ co-doped MXene electrode material as claimed in claim 1, wherein in step (1), the Lewis molten salt comprises NiCl 2 、CoCl 2 、ZnCl 2 、CdCl 2 、FeCl 2 、CuCl 2 AgCl, MXene insert metals include Ni, Co, Zn, Cd, Fe, Cu, Ag.
4. The preparation method of the metal-sulfur in-situ co-doped MXene electrode material according to any one of claims 1, wherein the sintering process in the tube furnace in the step (1) is carried out in an inert atmosphere at a calcination temperature of 500-1800 ℃, a heat preservation time of 3-24 h and a heating rate of 1-10 ℃/min.
5. The method for preparing the metal-sulfur in-situ co-doped MXene electrode material as claimed in any one of claims 1, wherein the sulfur-doped MAX and Lewis molten salt in step (2) have a molar ratio of 1: 1-1: 10.
6. the preparation method of the metal-sulfur in-situ co-doped MXene electrode material according to any one of claims 1 to 5, wherein the electrode material is applied to a power source of wearable devices, a micro supercapacitor, a metal ion battery (including lithium, sodium, potassium and aluminum ion batteries), a sodium-sulfur battery, a lithium-sulfur battery, a solid-state battery and a semi-solid-state battery.
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CN117534040A (en) * 2024-01-09 2024-02-09 北京师范大学 Multilayer titanium nitride material and preparation method thereof
CN117534040B (en) * 2024-01-09 2024-04-02 北京师范大学 Multilayer titanium nitride material and preparation method thereof

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