CN113233465B - V with filiform structure 2 C nanosheet and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a V with a filiform structure 2 C nanosheet and preparation method and application thereof, belonging to the technical field of lithium-sulfur batteries and alkali metal batteries 2 C controlling the hydrothermal reaction temperature to obtain V with a filiform structure 2 And C, the operation is simple, the requirement on equipment is not high, and industrial production can be realized. The obtained V wound with nano-wire 2 The C nanosheet is novel in structure, and the special structure can effectively adsorb polysulfide when used for a lithium-sulfur battery, so that the shuttle effect of the polysulfide in electrolyte is inhibited, the battery capacity is improved, the battery can be well maintained under a high multiplying power for a long time, and the C nanosheet has a good application prospect in the lithium-sulfur battery.
Description
Technical Field
The present invention belongs to a nano functional materialField, in particular to a V with a filiform structure 2 C nano sheet and preparation method and application thereof.
Background
Mxene phase by etching away the precursor M n+1 AX n A atoms in the phase being prepared, M n+1 AX n Is a general name of a ternary layered compound, wherein M represents early transition metals such as Ti, V, nb, mo, cr and the like; a represents a group III, IV element, such as: al, si; x represents C or N. V 2 C as a novel two-dimensional material Mxene has a very small band gap, so the material has good conductivity, shows metallic properties, and is widely applied to steel and hard alloy.
Due to V 2 The preparation of C is more difficult than other Mxenes, so that V is synthesized at present 2 Most of C is a simpler two-dimensional layered structure, and does not relate to a more complicated and more fine nano-belt wound nano-sheet structure. Meanwhile, the obtained structure has potential only to be applied to lithium-sulfur batteries in theory, but does not really show excellent performance enough to be used as a battery material.
Disclosure of Invention
The invention aims to provide a V with a filiform structure 2 The preparation method is simple to operate, has low requirements on equipment, and can be used for simply and efficiently preparing V with a filamentous structure 2 C nanosheet, V of the filamentous structure 2 The C nanosheet is novel in structure, and the special structure of the C nanosheet can effectively adsorb polysulfide and inhibit the shuttling effect of the polysulfide in electrolyte when the C nanosheet is used for a lithium-sulfur battery, so that the battery capacity is improved, and the battery capacity is better maintained.
Based on the purpose, the invention adopts the following technical scheme:
v with filiform structure 2 The preparation method of the C nano sheet comprises the following steps:
(1) Will V 2 Stirring AlC powder in hydrofluoric acid solution at normal temperature for etching, repeatedly cleaning with deionized water until pH is neutral after reaction, and vacuum filtering to obtain suspensionThe suspension is subjected to a freeze-drying machine to obtain a suspension V 2 C, first powder;
(2) Will V 2 C, adding the first powder and sodium alginate into a mixed solvent of deionized water and ethylenediamine to prepare a suspension, carrying out hydrothermal reaction on the suspension at 140-180 ℃, cooling after the reaction is finished, and centrifuging to obtain V with a filamentous structure 2 C nano-sheet.
Further, V in step (2) 2 The mass ratio of the first powder to the sodium alginate is 50, the volume ratio of the deionized water to the ethylenediamine is 10, and every 200mgV is as follows 2 C the first powder needs to be added with 3mL of ethylenediamine.
Further, the hydrothermal reaction time is 10 to 1697 hours.
V with filamentous structure prepared by the preparation method 2 C nanometer sheet.
V having a filament structure as described above 2 Application of C nanosheet in lithium-sulfur battery, namely applying V 2 Mixing the C nano sheet and pure sulfur according to the proportion of 7:3, preserving heat for 30min at 40 ℃, then preserving heat for 10h at 160 ℃ for carrying out sulfur to obtain a positive electrode material, uniformly mixing the obtained positive electrode material, acetylene black and PVDF according to the mass ratio of 7. Preferably, V 2 The load capacity of the C nano-sheet on the aluminum foil is 2.3 mg/cm 2 The drying refers to drying at 50 ℃ for 720 min. And (3) assembling the battery in a glove box by taking a lithium sheet as a negative electrode and taking a 1.0M LiTFSI DME/DOL solution as an electrolyte.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a V with a filamentous structure 2 C nanosheet and preparation method and application thereof. The preparation method obtains V with a filamentous structure by controlling reaction conditions and adding a certain proportion of ethylenediamine and sodium alginate 2 The C nanosheet is simple to operate, has low requirements on equipment, and can realize industrial production. V obtained thereby 2 The C nanosheet is novel in structure, and the special structure can effectively adsorb polysulfide and inhibit polysulfide when being used for a lithium-sulfur batteryThe shuttle effect of the sulfide in the electrolyte improves the battery capacity, better maintains the battery capacity, and has better application prospect in the lithium-sulfur battery.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows a V with a filamentous structure according to example 1 of the present invention 2 A scanning electron microscope image of the C nanosheet;
FIG. 2 shows a V with a filamentous structure according to example 2 of the present invention 2 C, scanning electron microscope image of the nanosheet;
FIG. 3 shows a V with a filamentous structure according to example 3 of the present invention 2 A scanning electron microscope image of the C nanosheet;
FIG. 4 shows a V having a filament-like structure according to comparative example 1 of the present invention 2 A transmission electron microscope image of the C nanosheet;
FIG. 5 shows a V of a filamentous structure provided in comparative example 2 of the present invention 2 C, transmission electron microscope image of the nanosheet;
FIG. 6 shows a V of a filamentous structure provided in comparative example 3 of the present invention 2 A transmission electron microscope image of the C nanosheet;
FIG. 7 shows a V of a filamentous structure provided in comparative example 4 of the present invention 2 C, transmission electron microscope image of the nanosheet;
FIG. 8 shows a V of a filamentous structure provided in comparative example 5 of the present invention 2 C, transmission electron microscope image of the nanosheet;
FIG. 9 shows V provided in example 1 of the present invention and comparative example 1 2 A performance diagram of a lithium-sulfur battery made of C nanosheets;
FIG. 10 shows V provided in example 1 of the present invention and comparative example 1 2 And C nanosheet prepared lithium sulfur battery stability graph.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The embodiment of the invention provides a V with a filamentous structure 2 C nano sheet and preparation method and application thereof. The preparation method controls the reaction conditions and adds a certain proportion of ethylenediamine and sodium alginate to obtain the V with a filiform structure 2 The C nanosheet is simple to operate, has low requirements on equipment, and can realize industrial production. V obtained thereby 2 The C nanosheet is novel in structure, and the special structure can effectively adsorb polysulfide when used for a lithium-sulfur battery, so that the shuttle effect of the polysulfide in electrolyte is inhibited, the battery capacity is improved, the battery capacity is better maintained, and the C nanosheet has a better application prospect in the lithium-sulfur battery.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
V with filiform structure 2 C nano sheet, its preparation method is as follows:
s1, taking 500mg V 2 Stirring AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly cleaning with deionized water until the pH value is 7 after the reaction is finished, and finally transferring the solution to a vacuum freeze dryer for drying for 48h at (-55 ℃), thus obtaining V 2 C, first powder;
s2. In N 2 Under protective atmosphere, 200mg of lyophilized V was taken 2 Dispersing C and 4mg Sodium Alginate (SA) in 30mL deionized water and 3mL ethylenediamine (more than or equal to 99.0%, AR, great), carrying out hydrothermal reaction on the suspension in a sealed polytetrafluoroethylene reaction kettle at 140 ℃ for 12h, cooling to room temperature after the reaction is finished, centrifuging, and then carrying out vacuum drying at 60 ℃ for 24h to obtain V with a filamentous structure 2 C nanosheet; it sweepsAs shown in FIG. 1, at adjacent V 2 A small number of nanoribbons can be observed between the C layers.
Example 2
V with filiform structure 2 C nano sheet, its preparation method is as follows:
s1, taking 500mg V 2 Stirring AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly cleaning with deionized water until the pH value is 7 after the reaction is finished, and finally transferring the solution to a vacuum freeze dryer for drying for 48h at (-55 ℃), thus obtaining V 2 C, first powder;
s2. In N 2 Under protective atmosphere, 200mg of lyophilized V was taken 2 Dispersing C and 4mg Sodium Alginate (SA) in 30mL deionized water and 3mL ethylenediamine (more than or equal to 99.0%, AR, great), carrying out hydrothermal reaction on the suspension in a sealed polytetrafluoroethylene reaction kettle at 160 ℃ for 12h, cooling to room temperature after the reaction is finished, centrifuging, and then carrying out vacuum drying at 60 ℃ for 24h to obtain V with a filamentous structure 2 C nanosheet; as shown in fig. 2, it can be seen that various nanobelts are generated, which tightly weaves the discrete nanosheets together to form an interconnected 3D structure.
Example 3
V with filiform structure 2 C nano sheet, its preparation method is as follows:
s1, taking 500mg V 2 Stirring the AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly cleaning the mixture with deionized water until the pH value is 7 after the reaction is finished, and finally transferring the mixture to a vacuum freeze dryer for drying for 48h at the temperature of-55 ℃ to obtain V 2 C, first powder;
s2. In N 2 Under protective atmosphere, 200mg of lyophilized V was taken 2 Dispersing C and 4mg of Sodium Alginate (SA) in 30mL of deionized water and 3mL ethylenediamine (more than or equal to 99.0%, AR, great), carrying out hydrothermal reaction on the suspension in a sealed polytetrafluoroethylene reaction kettle at 180 ℃ for 12h, cooling to room temperature after the reaction is finished, and carrying out vacuum drying at 60 ℃ for 24h after centrifugation to obtain black precipitate; the scanning electron micrograph is shown in FIG. 3, V 2 High C nanosheet at 180 DEG CAlmost disappears at temperature and instead is a rich population of inter-woven nanoribbons and some discrete distribution of nano-flakes.
Comparative example 1
This comparative example provides a layered V 2 The preparation method of the C nanosheet is basically the same as that of example 1, except that the hydrothermal time is shortened to 4h, and the scanning electron microscope and the transmission electron microscope are respectively shown in fig. 4a and 4b, so that the original V is shown 2 No obvious morphological change is seen in C nanoplatelets compared to C nanoplatelets, which means that the morphological change needs to overcome a certain reaction barrier.
Comparative example 2
This comparative example provides a layered V 2 C nano-sheet, the preparation method is the same as that of example 1, the difference is that the hydrothermal time is shortened to 8h, the scanning electron microscope is shown as figure 5a, and the transmission electron microscope is shown as figure 5b, and the accordion V can be seen 2 The edges and surfaces of the C-nanosheets form a plurality of nanoribbons having a width of less than 20 nm, forming an interconnected 3D structure.
Comparative example 3
This comparative example provides a layered V 2 C nanosheet, the preparation method thereof is the same as that of example 1, except that the hydrothermal time is prolonged to 16h, the scanning electron microscope is shown as figure 6a, and the transmission electron microscope is shown as figure 6b, and V can be seen 2 The C-nanoplatelets have become intertwined filamentous nanoribbons.
Comparative example 4
This comparative example provides a layered V 2 C nano sheet, the preparation method is the same as that of example 1, except that the hydrothermal time is prolonged to 24h, the scanning electron microscope is shown as figure 7a, and the transmission electron microscope is shown as figure 7b, and a large number of nano belts with different sizes are attached to the gauze-shaped V 2 C, the surface of the nanosheet.
Comparative example 5
This comparative example provides a layered V 2 C nanosheets, the preparation method of which is the same as in example 1, except that the hydrothermal time is prolonged to 30h, and the transmission electron microscope thereof is shown in fig. 8a and 8b, it can be seen that some nanodots are still present on the nanobelts.
Test example 1
V using example 1~3 and comparative example 1~5 2 And C, observing and recording the structural shape under an electron microscope, wherein the recording result is shown in Table 1.
TABLE 1 layered filaments V 2 C nano sheet structure shape contrast
As can be seen from Table 1, V with different morphologies can be obtained by controlling the hydrothermal reaction time at the same hydrothermal temperature 2 C nanoplatelets, which present a shearing mechanism mediated by SA to form filamentous structures. Under the alkalescent environment (the function of the ethylenediamine), SA is rich in functional groups, is a linear polysaccharide rich in carboxyl/hydroxyl, can be used as a reaction igniter in beta-D mannuronic acid units and alpha-L guluronic acid units, and is V 2 The delamination and fracture of the C nanosheets provide a powerful driver. V 2 Edge V atom and V of C surface 2 Extensive hydrogen bonding between C and SA can weaken the adjacent V 2 The V-C bonds and van der Waals forces between the C nanoplatelets. The SA does not completely exert a shearing effect at the reaction temperature of 140 ℃ so that a few nanobelts are generated, the SA sufficiently exerts the shearing effect at the reaction temperature of 160 ℃, so that the obvious nanobelts are generated, and the nanobelts are denatured into nano fragments and even nano dots at the reaction temperature of 180 ℃. Furthermore, the application also carries out the step of changing the time of the hydrothermal reaction when the hydrothermal temperature of 160 ℃ is kept constant for V 2 An exploration experiment for the influence of the morphology of the C nanosheet can be found from comparative example 1 to comparative example 3 that nanobelts are gradually generated by increasing the time, but when the time is increased to 16h and then the hydrothermal reaction time is increased, from comparative example 4 and comparative example 5, V can be found 2 The nanosheets of C have been destroyed.
Test example 2
V with filamentous Structure prepared by example 1 2 C nanosheet, and V prepared in comparative example 1 without filamentous structure 2 C nanosheets, each beingThe carrier is a positive electrode sulfur carrier, is applied to a lithium sulfur battery, and the performance of the lithium sulfur battery is tested, and the test results are shown in table 2, wherein the lithium sulfur battery is manufactured by the following process: v obtained in example 1 2 C nanosheet or layered V made in comparative example 1 2 Mixing the C nanosheet with pure sulfur (Aladdin, the purity is more than or equal to 99.99%) according to the mass ratio of 7:3, preserving the heat at 40 ℃ for 30min, and then reacting at 160 ℃ for 10h to carry out sulfur, thus obtaining the anode material. Preferably, said layered V 2 When the C nano-sheets react with the pure sulfur, the temperature is raised to 40 ℃ from room temperature at the rate of 1~3 ℃/min, the temperature is kept at 40 ℃ for 30min, and then the temperature is raised to 160 ℃ at the rate of 3 ℃/min and kept at 10 h.
And (2) uniformly mixing the obtained positive electrode material with acetylene black and PVDF according to a mass ratio of 7 2 The surface loading of the C nano-sheets is 2.3 mg/cm 2 And standing in an oven at 50 ℃ for 720 min to obtain the positive plate. Lithium plate (diameter 0.8 cm) as cathode, 1.0M DME/DOL (volume ratio 1:1) of LiTFSI with 2.0 wt% LiNO 3 The electrolyte is used, and the battery is assembled in a glove box, and the charging and discharging voltage is 2.8V-1.6V (vs + ) The charge-discharge current density was 0.5C. The performance graph and stability graph of the lithium sulfur battery are shown in fig. 9 and 10, and the results of fig. 9 and 10 are shown in table 2.
TABLE 2 comparison of lithium-sulfur cell Performance
As can be seen from Table 2, V having a filamentous structure provided by the examples of the present invention 2 The initial discharge capacity of the lithium-sulfur battery prepared by the C nanosheet is up to 1360 mAh g under 0.1C -1 (as shown in FIG. 9), has very close to the theoretical capacity of a lithium-sulfur battery of 1675 mAh g -1 . In contrast, comparative example 1V without filamentary structures 2 The capacity of the C nano sheet is much smaller, and is only 1050 mAh & g -1 . As shown in FIG. 10, the capacity of example 1 after 100 cycles at 0.5C was maintained at 820 mAh g -1 In contrast, comparative example 1 had only 408 mAh g -1 . Should be the electrolyte penetrate into V having a filamentous structure 2 In the C nano sheet structure, polysulfide generated in the charging and discharging process is subjected to the double adsorption effect of the nano belt and the nano sheet, and the shuttle effect of the polysulfide is inhibited, so that the polysulfide has the capacity of better keeping the battery capacity.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. V with filiform structure 2 Use of C nanoplates in lithium sulphur batteries, characterised in that V has a filamentous structure 2 The C nanosheet is obtained by the following process: (1) Will V 2 Stirring AlC powder in hydrofluoric acid solution at normal temperature for etching, repeatedly cleaning with deionized water until pH is neutral after reaction, vacuum-filtering to obtain suspension, and freeze-drying to obtain V 2 C, first powder;
(2) In N 2 Under a protective atmosphere, adding V 2 C, adding the first powder and sodium alginate into a mixed solvent of deionized water and ethylenediamine to prepare a suspension, carrying out hydrothermal reaction on the suspension at 140-180 ℃, cooling after the reaction is finished, and centrifuging to obtain V with a filamentous structure 2 C nanosheet; v in step (2) 2 The mass ratio of the first powder to the sodium alginate is 50, the volume ratio of the deionized water to the ethylenediamine is 10, and every 200mgV is as follows 2 C, 3mL of ethylenediamine needs to be added into the first powder;
the time of the hydrothermal reaction is 10 to 1697 h,
will V 2 Mixing the C nanosheet with sulfur according to the proportion of 7:3, carrying out sulfur loading to obtain a positive electrode material, uniformly mixing the obtained positive electrode material with acetylene black and PVDF according to the mass ratio of 7; v 2 The loading capacity of the C nano-sheets on the aluminum foil is 2.3 mg/cm 2 The drying refers to drying for 720 min at 50 ℃; the sulfur carrying means that the sulfur carrying is carried out by firstly preserving the heat at 40 ℃ for 30min and then preserving the heat at 160 ℃ for 10 h.
2. The use of claim 1, wherein the battery is assembled in a glove box using a lithium plate as the negative electrode and 1.0M LiTFSI DME/DOL solution as the electrolyte.
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| A hydrothermal etching route to synthesis of 2D MXene (Ti3C2, Nb2C): Enhanced exfoliation and improved adsorption performance;Peng,C;《 CERAMICS INTERNATIONAL》;20181015;第44卷(第15期);全文 * |
| Ti2C MXene Modified with Ceramic Oxide and Noble Metal Nanoparticles: Synthesis, Morphostructural Properties, and High Photocatalytic Activity;Wojciechowski,T;《INORGANIC CHEMISTRY》;20190603;第58卷(第11期);全文 * |
| Ultrafine Ti3C2 MXene nanodots-interspersed nanosheet for high-energy-density lithium-sulfur batteries;Xiao,ZB;《ACS NANO》;20190313;第13卷(第3期);实验部分 * |
| 二维材料MXene及其超级电容器的研究进展;潘召朴;《微纳电子技术》;20210209;全文 * |
| 超薄MoS_2纳米片改性隔膜用于锂硫电池的研究;李娇娇等;《燕山大学学报》;20191130(第06期);全文 * |
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