CN114843510B - 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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CN114843510B
CN114843510B CN202110131203.4A CN202110131203A CN114843510B CN 114843510 B CN114843510 B CN 114843510B CN 202110131203 A CN202110131203 A CN 202110131203A CN 114843510 B CN114843510 B CN 114843510B
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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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    • H01—ELECTRIC ELEMENTS
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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 carrying out element replacement on an A phase of S-MAX through Lewis molten salt reaction to synthesize a metal-embedded nano lamellar MAX phase, and then etching and extracting an A metal atomic layer in the MAX phase material by a chemical etching method to prepare the two-dimensional lamellar nano material MXene. The independent electrode material with high capacity and long service life, which is designed by the invention, can effectively solve the great limitation of the shuttle effect of lithium polysulfide (LiPS), and is important for developing advanced 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, concerns have arisen about lithium batteries due to the high cost and availability of lithium resources. The room temperature sodium-sulfur battery and the lithium-sulfur battery have development prospect due to the advantages of high theoretical energy density, large sodium-lithium-sulfur reserves, low cost and the like. However, sodium-sulfur batteries and lithium-sulfur batteries have the disadvantages of low reversible capacity, poor self-discharge and cycle performance and the like, and the wide application of the sodium-sulfur batteries and the lithium-sulfur batteries is hindered. The natural insulating nature of elemental sulfur limits its use as an active material, resulting in slow electrochemical process kinetics at the cathode. Meanwhile, the solubility of the reduced sodium polysulfide in the charge and discharge process is more serious than that of lithium polysulfide, so that the uncontrollable shuttle effect of the sodium polysulfide is increased, and the cycle life of the sodium-sulfur battery is poor. Due to its two-dimensional structure, functional surface, high conductivity and chemical durability of the battery, MXenes has wide application prospects in 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, lithium sulfur batteries use abundant elements, providing an attractive alternative to currently used batteries, but they require better sulfur-containing materials to compete for capacity and cycling capability with lithium ion batteries. The invention provides an in-situ sulfur doping strategy for functionalizing an MXene nano-sheet by introducing hetero-atomic sulfur from a MAX precursor, co-doped metal (M) into the MXene structure. And preparing the three-dimensional wrinkled MXene nano structure with high specific surface area by adopting a vacuum freeze drying method. In the sodium-sulfur battery and the lithium-sulfur battery at room temperature, a specially-made shrinkage sulfur doped MXene (M, S-MXene) nanosheet is adopted as an electrode main body material. M, S-MXene is highly polar with sodium polysulfide and lithium polysulfide, limiting the diffusion of sodium polysulfide and lithium polysulfide.
In view of this, the present invention has been made.
Disclosure of Invention
The first object of the present invention is to provide a metal-sulfur in-situ co-doped MXene electrode material, which can be used as a positive electrode material or a negative electrode material, and has the advantages of improving specific capacity, stabilizing battery performance, prolonging battery life and the like when applied to the battery field.
A second object of the present invention is to provide applications of MXene electrode materials, which are very broad, 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 invention is not limited in its application.
In order to achieve the first object of the present invention, the following technical solutions are specifically adopted:
the preparation method of the metal-sulfur in-situ co-doped MXene electrode material comprises the following specific steps:
firstly, mixing titanium, aluminum, graphite and sulfur in a certain atomic ratio to synthesize the polycrystalline sulfur doped MAX powder. 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. A 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. In a glove box, the starting materials were thoroughly mixed with a mortar under nitrogen protection. The resulting mixture powder was then taken out of the glove box and put into an alumina crucible. The alumina crucible is charged into a tube furnace and calcined under the protection of an inert atmosphere. After the reaction, the product was washed with deionized water to remove residual molten salt, and the final product was dried. Finally, the metal-sulfur in-situ co-doped MXene material is obtained.
Preferably, the MAX phase comprises any one or more than two MAX phase ceramic combinations of Ti2AlC、Ti2AlN、V2AlC、V2AlN、Nb2AlC、NbAl2N、Ta2AlC、Ti3AlC2、Ti3AlN2、V3AlC2、Ta3AlC2、Ta3AlN2、 Ti4AlC3、Ti4AlN3、Ta4AlC3、Ta4NAl3、Nb4AlC3 ;
Preferably, the MXene comprises Sc2C、Sc2N、Ti2C、Ti2N、V2C、V2N、Cr2C、Cr2N、Zr2C、Zr2N、Nb2C、Nb2N、Hf2C、Hf2N、Ta2C、Mo2C、Ti3C2、Ti3N2、V3C2、Ta3C2、Ta3N2、Mo3C2、(Mo4V)C4、(Cr2/3Ti1/2)3C2、Ti4C3、Ti4N3、V4C3、V4N3、Ta4C3、Ta4N3、Nb4C3, or a combination thereof;
preferably, the sintering tube is a quartz tube of a high-temperature tube furnace, and the calcination temperature can reach 1650 ℃;
Preferably, the inert atmosphere is argon;
Preferably, the sulfur is doped into a mixture of titanium, aluminum, graphite and sulfur which are uniformly mixed according to different atomic ratios;
preferably, the sulfur-doped MAX-phase powder is present in a stoichiometric molar ratio with lewis molten salt of 1: 1-1: 10, mixing;
Preferably, the MXene embedded metal comprises Ni, co, zn, cd, fe, cu, ag;
preferably, the reaction centrifugation is carried out for 5-15 min at a speed of 3000-6000 rpm;
Preferably, the reaction drying is specifically vacuum drying at 30-80 ℃ for 6-24 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) Sulfur is incorporated into the cathode body during the fabrication of lithium sulfur battery cathode materials, which body itself has high electron conductivity, excellent mechanical flexibility, and rich sites of chemical interaction. Forming a protective barrier in situ on the robust conductive cathode during cycling to fix polysulfide shuttling not only improves sulfur utilization but also greatly simplifies manufacturing processes;
(2) The sulfur-doped MXene electrode material can effectively relieve the problems that the cycle performance of a lithium-sulfur battery is poor, the utilization rate of active materials is low, and polysulfide and volume expansion limit the use of the lithium-sulfur battery and a 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 batteries and the like, and widens the application field of the MXene material.
Drawings
Fig. 1 is an SEM image of metal particles uniformly dispersed on Ti 3C2.
FIG. 2 is a pictorial view of various electrode materials, (a) a metal-sulfur in situ co-doped MXene ink and clay; (2) a flexible electrode material; (3) Nickel electrode material.
Detailed Description
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
First, titanium, aluminum, graphite, and sulfur were mixed in a certain atomic ratio to synthesize a polycrystalline sulfur-doped MAX powder (Ti 3AlC2Sx). The powder mixture was sintered in a high temperature tube furnace at 1650 ℃ in flowing argon. The heating rate was 5℃/min. The MAX product produced was ground and sieved through a 200 mesh screen. Sulfur-doped MAX phase powder (Ti 3AlC2Sx) (particle size <74 μm) was obtained. To synthesize the metal intercalation MAX phase, first MAX to CoCl 2 molten salt molar ratio 1:6 mixing the powders as starting materials. In a glove box, the starting materials were thoroughly mixed with a mortar under nitrogen protection. The resulting mixture powder was then taken out of the glove box and put into an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated under argon at 700 ℃ for 24 h. 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 3C2) was obtained.
Example 2
Preparation of metal-sulfur in-situ co-doped MXene electrode material
First, titanium, aluminum, graphite, and sulfur were mixed in a certain atomic ratio to synthesize a polycrystalline sulfur-doped MAX powder (Ti 3AlC2Sx). The powder mixture was sintered in a high temperature tube furnace at 1650 ℃ in flowing argon. The heating rate was 5℃/min. The MAX product produced was ground and sieved through a 200 mesh screen. Sulfur-doped MAX phase powder (Ti 3AlC2Sx) (particle size <74 μm) was obtained. To synthesize the metal intercalation MAX phase, first the MAX to NiCl 2 molten salt mole ratio 1:6 mixing the powders as starting materials. In a glove box, the starting materials were thoroughly mixed with a mortar under nitrogen protection. The resulting mixture powder was then taken out of the glove box and put into an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated under argon at 700 ℃ for 24 h. After the reaction, the product was washed with deionized water to remove residual NiCl 2, and the final product was dried at 40 ℃. Finally, a Ni-S co-doped MXene material (Ni, S-Ti 3C2) was obtained.
Example 3
Preparation of metal-sulfur in-situ co-doped MXene electrode material
First, titanium, aluminum, graphite, and sulfur were mixed in a certain atomic ratio to synthesize a polycrystalline sulfur-doped MAX powder (Ti 3AlC2Sx). The powder mixture was sintered in a flowing argon gas in a high temperature tube furnace at 1600 ℃. The heating rate was 5℃/min. The MAX product produced was ground and sieved through a 200 mesh screen. Sulfur-doped MAX phase powder (Ti 3AlC2Sx) (particle size <74 μm) was obtained. To synthesize the metal intercalation MAX phase, first MAX to CoCl 2、NiCl2 molten salt molar ratio 1:3:3 mixing the powder as starting material. In a glove box, the starting materials were thoroughly mixed with a mortar under nitrogen protection. The resulting mixture powder was then taken out of the glove box and put into an alumina crucible. The alumina crucible was charged into a tube furnace and heat treated under argon at 700 ℃ for 24 h. After the reaction, the product was washed with deionized water to remove residual CoCl 2、NiCl2, and the final product was dried at 40 ℃. Finally, co, ni, S Co-doped MXene material (Co, ni, S-Ti 3C2) was obtained.
Finally, it is noted that the above-mentioned preferred embodiments are only intended to illustrate rather than limit the invention, and that, although the invention has been described in detail by means of the above-mentioned preferred embodiments, 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 scope of the invention as defined by the appended claims.

Claims (2)

1. A method for preparing a metal-sulfur in-situ co-doped MXene electrode material, which is characterized by comprising the following steps:
Firstly mixing titanium, aluminum, graphite and sulfur in a certain atomic ratio to synthesize MAX powder doped with polycrystalline sulfur, sintering the powder mixture in a high-temperature tube furnace in flowing argon, wherein the sintering in the tube furnace is carried out under inert atmosphere, the calcining temperature is 500-1800 ℃, the heat preservation time is 3-24 h, the heating rate is 1-10 ℃/min,
Grinding the prepared MAX product, and sieving through a 200-mesh screen 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 raw materials in a glove box under the protection of nitrogen, taking out the obtained mixture powder from the glove box, placing the obtained mixture powder into an alumina crucible, placing the alumina crucible into a tubular furnace, calcining at 700 ℃ under the protection of inert atmosphere, washing a product with deionized water to remove residual molten salt after reaction, drying a final product, and finally obtaining the metal-sulfur in-situ co-doped MXene material;
The Lewis molten salt is one or more of NiCl 2、CoCl2、ZnCl2、CdCl2、FeCl2、CuCl2 and AgCl, and the MXene embedded metal is one or more of Ni, co, zn, cd, fe, cu, ag;
The molar ratio of the sulfur doped MAX to the Lewis molten salt is 1:1 to 1:10.
2. The method for preparing the metal-sulfur in-situ co-doped MXene electrode material according to claim 1, wherein the application range of the electrode material comprises a power supply of a wearable device, a micro super capacitor, a metal ion battery, a sodium-sulfur battery, a lithium-sulfur battery, a solid-state battery or a semi-solid battery.
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