CN113247902B - Preparation method and application of ionic liquid derived carbon crosslinked MXene three-dimensional network material - Google Patents
Preparation method and application of ionic liquid derived carbon crosslinked MXene three-dimensional network material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of an ionic liquid derived carbon crosslinked MXene three-dimensional network material. The MXene-based three-dimensional cross-linked network prepared by the method reserves good conductivity and large specific surface area, and has the characteristics of high pore volume, high number of exposed active sites, stable structure and the like. In addition, after high-temperature carbonization, the electrochemical active center is further enriched by the presence of oxygen and the heteroatom contained in the ionic liquid derived carbon, and the prepared three-dimensional cross-linked network material can show excellent high-load performance, rate capability and cycling stability when the anode of the lithium-sulfur battery is modified.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur battery electrode materials, and particularly relates to a preparation method and application of an ionic liquid derived carbon crosslinked MXene three-dimensional network material.
Background
Lithium ion batteries dominate power cells with an average energy density of about 260 Wh/kg, already approaching the theoretical limit (350 Wh/kg). The theoretical energy density of the lithium-sulfur battery is as high as 2600 Wh/kg, which is far higher than that of a commercial lithium ion battery, in addition, the sulfur resource is rich, the advantages of environmental protection and cost are achieved, the sulfur is easy to sublimate, the recovery of the lithium-sulfur battery is relatively simple and convenient in the future, and the advantages enable the lithium-sulfur battery to become a powerful competitor of a new generation of power source. However, the lithium-sulfur battery industrialization process still faces many obstacles, such as low sulfur conductivity, significant volume effect during charging and discharging, shuttle effect of lithium polysulfide, etc., thus resulting in relatively poor rate performance and cycle stability of the lithium-sulfur battery, and especially the requirement of high sulfur loading (> 70%) for practical application further aggravates these effects.
In recent years, researchers have designed and developed various three-dimensional porous carbon materials, such as carbon nanotubes, hollow carbon spheres, hierarchical porous carbon, and the like, so as to improve the utilization rate of sulfur and limit the migration of lithium polysulfide. However, the interaction between nonpolar carbon and polar lithium polysulfides is weak, and it is difficult to maintain stable capacity for a long period of time by relying only on physical constraints. The research finds that MXene serving as a novel two-dimensional metal carbon/nitride has the advantages of polarity, metal conductivity, excellent mechanical stability and the like, and is a high-performance lithium-sulfur battery positive electrode material with great application potential. However, two-dimensional materials are prone to stacking, resulting in a loss of active area and difficulty in achieving high sulfur loading. In order to construct a three-dimensional porous MXene structure with high sulfur carrying capacity, a sacrificial template is usually introduced or compounded with a three-dimensional carbon skeleton material (such as graphene, carbon nanotubes and the like). However, the three-dimensional porous structure obtained by the former has poor structural stability due to electrostatic repulsion between the two-dimensional nano sheets; the latter realizes the synergistic coupling among different components, but also dilutes the active site density of MXene, and weakens the chemical sulfur fixation capacity of the whole electrode material. Therefore, the MXene-based three-dimensional porous material with high-density active sites and stable structure is constructed, and the method has important significance for developing the lithium-sulfur battery with high specific capacitance and stability.
Disclosure of Invention
The invention solves the technical problem of providing a preparation method and application of an MXene three-dimensional network material crosslinked by ionic liquid derived carbon, and provides a simple and green new method for preparing the MXene three-dimensional crosslinked network material with high-density active sites and stable structure based on covalent interaction between the ionic liquid and the MXene.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the ionic liquid derived carbon crosslinked MXene three-dimensional network material is characterized by comprising the following specific steps:
step S1: mixing MAX phase precursor with acid etching solution, continuously stirring until the reaction is complete, centrifuging the obtained solution, washing with water to neutrality, dispersing in water to obtain MXene suspension, and freeze-drying to obtain MXene powder sample, wherein the MAX phase precursor is Ti3AlC2Or Ti2Al, MXene powder sample obtained after etching corresponds to Ti3C2Or Ti2C, acid etching liquid is lithium fluoride-hydrochloric acid mixed solution;
step S2: preparing an MXene powder sample obtained in the step S1 and deionized water into an MXene dispersion liquid, adding an ionic liquid for mixing, and treating the mixed solution at 35-100 ℃ for 3-24 hours to obtain hydrogel, wherein the ionic liquid is tetrafluoroborate, hexafluorophosphate or hexafluoroantimonate;
step S3: and (4) carrying out freeze drying treatment on the hydrogel obtained in the step (S2), and carrying out heat treatment on the freeze-dried product at 400-800 ℃ under the protection of inert gas to obtain the ionic liquid derived carbon crosslinked MXene three-dimensional network material.
Further limiting, in the step S1, the MAX phase precursor and the acid etching solution are reacted at the temperature of 30-90 ℃ for 20-40 h.
Further, the concentration of the MXene dispersion in the step S2 is 5-15 g/L.
Further limiting, in the step S2, the feeding molar ratio of MXene to the ionic liquid is 10: 1-1: 1.
Further, the temperature of the freeze-drying in the step S3 is-60 ℃, and the time of the freeze-drying is 24 h.
The ionic liquid derived carbon crosslinked MXene three-dimensional crosslinked network material prepared by the preparation method is used for the positive electrode material of the lithium-sulfur battery.
Compared with the prior art, the invention has the following beneficial effects: the invention utilizes the pi-pi interaction of ionic liquid and MXene to introduce the ionic liquid into a two-dimensional MXene layer, the ionic liquid is further chemically bonded with oxygen-containing functional groups on the surface of MXene to initiate crosslinking and form gel, the hydrogel is frozen, dried and thermally treated, the ionic liquid is converted into a heteroatom doped carbon material, the hydroxyl group and the oxygen-containing functional group grafted on the surface of MXene slightly oxidize the surface of MXene, and the hydroxyl group and the oxygen-containing functional group are chemically bonded to finally obtain the heteroatom doped carbon crosslinked MXene three-dimensional network material. The prepared MXene-based three-dimensional cross-linked network material keeps good conductivity and large specific surface area, and has the characteristics of high pore volume, high number of exposed active sites, stable structure and the like. In addition, the electrochemical active center is further enriched by the existence of oxygen element and the heteroatom contained in the ionic liquid derived carbon. Based on the advantages, the high load performance, rate capability and cycling stability of the heteroatom-doped carbon crosslinked MXene three-dimensional network material prepared by the method are remarkably improved when the positive electrode of the lithium-sulfur battery is modified.
Drawings
FIG. 1 is a representation of the hexafluoroantimonate-derived carbon crosslinked Ti of example 13C2SEM image of three-dimensional network gel;
FIG. 2 is a carbon-crosslinked Ti derived from tetrafluoroborate in example 23C2SEM image of three-dimensional network gel;
FIG. 3 is the hexafluorophosphate derived carbon crosslinked Ti of example 32C, SEM image of three-dimensional network gel;
FIG. 4 is the hexafluoroantimonate-derived carbon crosslinked Ti of example 13C2The three-dimensional network material is used as a rate performance schematic diagram of a lithium-sulfur battery cathode material;
FIG. 5 is the hexafluoroantimonate-derived carbon crosslinked Ti of example 13C2The three-dimensional network material is used as a cycle performance diagram of the lithium-sulfur battery cathode material.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
This example hexafluoroantimonate-derived carbon crosslinked Ti3C2The preparation method of the three-dimensional network material comprises the following steps:
(1) mixing 1 g of Ti3AlC2With 1 g of lithium fluoride and 25 mL of 9 mol L-1Mixing the mixed solution of hydrochloric acid, continuously stirring for 30 h at 35 ℃ until the reaction is complete, centrifugally washing the obtained solution to be neutral, and dispersing the solution in water to obtain Ti3C2The suspension is frozen and dried to obtain Ti3C2A powder sample;
(2) ti obtained in the step (1)3C2Powder samples were dosed with deionized water to 10 g L-1Ti of (A)3 C 210 mL of Ti was taken as a dispersion3C20.046 g of 1-butyl-3-methylimidazolium hexafluoroantimonate was added to the dispersion and mixed (molar ratio-Ti)3C21-butyl-3-methylimidazolium hexafluoroantimonate =5:1), and treating the mixed solution at 100 ℃ for 3 hours to prepare the hydrogel.
(3) Freezing and drying the hydrogel obtained in the step (2), and carrying out heat treatment on the product after cold drying at 400 ℃ under the protection of inert gas to obtain the ionic liquid derived carbon crosslinked Ti3C2A three-dimensional network material.
FIG. 1 is a schematic representation of hexafluoroantimonate-derived carbon crosslinked Ti as provided in the examples herein3C2According to the SEM image of the three-dimensional network gel, the prepared composite material forms a three-dimensional network structure, and is stable in structure and not easy to collapse. FIG. 4 is the hexafluoroantimonate-derived carbon crosslinked Ti of example 13C2The rate performance of the three-dimensional network material used as the positive electrode material of the lithium-sulfur battery is shown in the figure, and the hexafluoroantimonate derived carbon crosslinked Ti3C2The first-circle discharge capacity of the three-dimensional network material 0.1C reaches 1150 mAh g-1And the capacity can still reach after the circulation of 700 circles under the current density of 2C570.6 mAh g-1。
Example 2
This example tetrafluoroborate-derived carbon crosslinked Ti3C2The preparation method of the three-dimensional cross-linked network material comprises the following steps:
(1) mixing 1 g of Ti3AlC2With 1 g of lithium fluoride and 25 mL of 9 mol L-1Mixing the mixed solution of hydrochloric acid, continuously stirring for 30 h at 35 ℃ until the reaction is complete, centrifugally washing the obtained solution to be neutral, and dispersing the solution in water to obtain Ti3C2The suspension is frozen and dried to obtain Ti3C2Powder sample;
(2) ti obtained in the step (1)3C2Powder samples were dosed with deionized water to 10 g L-1Ti of (A)3 C 210 mL of Ti was taken as a dispersion3C20.024 g of 1-butyl-3-methylimidazolium tetrafluoroborate (molar ratio-Ti) is added to the dispersion3C21-butyl-3-methylimidazole tetrafluoroborate =10:1), and treating the mixed solution at 35 ℃ for 24 hours to prepare hydrogel;
(3) freezing and drying the hydrogel obtained in the step (2), and carrying out heat treatment on the product after cold drying at 600 ℃ under the protection of inert gas to obtain the tetrafluoborate derived carbon crosslinked Ti3C2A three-dimensional network material.
FIG. 2 is a carbon-crosslinked Ti derived from tetrafluoroborate in example 23C2SEM image of three-dimensional network gel, which shows tetrafluoroborate and Ti3C2And crosslinking to form a three-dimensional network structure.
Example 3
This example hexafluorophosphate derived carbon crosslinked Ti2The preparation method of the C three-dimensional network material comprises the following steps:
(1) 1 g of Ti2AlC with 1 g of lithium fluoride and 25 mL of 9 mol L-1Mixing the mixed solution of hydrochloric acid, continuously stirring for 30 h at 35 ℃ until the reaction is complete, centrifugally washing the obtained solution to be neutral, and dispersing the solution in water to obtain Ti2C, freeze drying to obtain Ti2C, sampling powder;
(2) will step withTi obtained in step (1)2C powder sample and deionized water are prepared into 10 g L-1Ti of (A)2C dispersion, 10 mL of Ti was taken2C Dispersion 0.114 g of 1-butyl-3-methylimidazolium hexafluorophosphate (molar ratio-Ti) was added2C, 1-butyl-3-methylimidazolium hexafluorophosphate =1:1), and treating the mixed solution at 60 ℃ for 6 h to prepare hydrogel;
(3) freezing and drying the hydrogel obtained in the step (2), and carrying out heat treatment on the product after cold drying at 800 ℃ under the protection of inert gas to obtain hexafluorophosphate derived carbon crosslinked Ti2C, three-dimensional network material.
FIG. 3 is the hexafluorophosphate derived carbon crosslinked Ti of example 32SEM image of C three-dimensional network gel, showing hexafluorophosphate and Ti2C, forming a three-dimensional network structure through crosslinking.
Example 4
This example hexafluoroantimonate-derived carbon crosslinked Ti2The preparation method of the C three-dimensional network material comprises the following steps:
(1) mixing 1 g of Ti2AlC with 1 g of lithium fluoride and 25 mL of 9 mol L-1Mixing the mixed solution of hydrochloric acid, continuously stirring for 24 h at 80 ℃ until the reaction is complete, centrifugally washing the obtained solution to be neutral, and dispersing the solution in water to obtain Ti2C, freeze drying to obtain Ti2C, sampling powder;
(2) ti obtained in the step (1)2C powder sample and deionized water are prepared into 10 g L-1Ti of (A)2C dispersion, 5 mL of Ti was taken2C the dispersion was mixed by adding 0.115 g of 1-butyl-3-methylimidazolium hexafluoroantimonate (molar ratio-Ti)2C: 1-butyl-3-methylimidazolium hexafluoroantimonate =2:1), and treating the mixed solution at 80 ℃ for 4 hours to prepare hydrogel;
(3) freezing and drying the hydrogel obtained in the step (2), and carrying out heat treatment on the product after cold drying at 400 ℃ under the protection of inert gas to obtain the ionic liquid derived carbon crosslinked Ti2C, three-dimensional network material.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (4)
1. The preparation method of the ionic liquid derived carbon crosslinked MXene three-dimensional network material is characterized by comprising the following specific steps of:
step S1: mixing MAX phase precursor with acid etching solution, continuously stirring at 30-90 ℃ for reaction for 20-40 h until the reaction is complete, centrifuging the obtained solution, washing to be neutral, dispersing in water to obtain MXene suspension, and freeze-drying to obtain MXene powder sample, wherein the MAX phase precursor is Ti3AlC2Or Ti2Al, MXene powder sample obtained after etching corresponds to Ti3C2Or Ti2C, acid etching liquid is lithium fluoride-hydrochloric acid mixed solution;
step S2: preparing an MXene powder sample obtained in the step S1 and deionized water into an MXene dispersion liquid, adding an ionic liquid for mixing, and treating the mixed solution at 35-100 ℃ for 3-24 hours to obtain hydrogel, wherein the ionic liquid is tetrafluoroborate, hexafluorophosphate or hexafluoroantimonate, and the feeding molar ratio of MXene to the ionic liquid is 10: 1-1: 1;
step S3: and (4) carrying out freeze drying treatment on the hydrogel obtained in the step (S2), and carrying out heat treatment on the freeze-dried product at 400-800 ℃ under the protection of inert gas to obtain the ionic liquid derived carbon crosslinked MXene three-dimensional network material.
2. The preparation method of the ionic liquid derived carbon crosslinked MXene three-dimensional network material according to claim 1, wherein: the concentration of the MXene dispersion liquid in the step S2 is 5-15 g/L.
3. The preparation method of the ionic liquid derived carbon crosslinked MXene three-dimensional network material according to claim 1, wherein: the temperature of the freeze drying in the step S3 is-60 ℃, and the time of the freeze drying is 24 h.
4. The ionic liquid derived carbon crosslinked MXene three-dimensional crosslinked network material prepared by the method according to any one of claims 1 to 3 is used as a positive electrode material of a lithium-sulfur battery.
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