CN113233465A - V with filiform structure2C nanosheet and preparation method and application thereof - Google Patents

V with filiform structure2C nanosheet and preparation method and application thereof Download PDF

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CN113233465A
CN113233465A CN202110512124.8A CN202110512124A CN113233465A CN 113233465 A CN113233465 A CN 113233465A CN 202110512124 A CN202110512124 A CN 202110512124A CN 113233465 A CN113233465 A CN 113233465A
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肖助兵
徐梦瑶
吴天利
周丹
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Henan University
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Abstract

The invention discloses a V with a filiform structure2C nanosheet and preparation method and application thereof, belonging to the technical field of lithium-sulfur batteries and alkali metal batteries2C controlling the hydrothermal reaction temperature to obtain V with a filiform structure2C, it is not only simple to operate, but also has no requirements for equipmentHigh efficiency, and can realize industrialized production. The obtained nanowire-wound V2The 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

With filamentary structureV2C nanosheet and preparation method and application thereof
Technical Field
The invention belongs to the field of nano functional materials, and particularly relates to a V with a filamentous structure2C nanosheet and preparation method and application thereof.
Background
Mxene phase by etching away the precursor Mn+1AXnFrom A atoms in phase, Mn+1AXnIs 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. V2C 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 V2The preparation of C is more difficult than other Mxenes, so that V is synthesized at present2Most 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 structure2The preparation method is simple to operate, has low requirements on equipment, and can be used for simply and efficiently preparing V with a filamentous structure2C nanosheet, V of the filamentous structure2The C nanosheet is novel in structure, and the special structure of the C nanosheet can effectively adsorb polysulfide when the C nanosheet is used for a lithium-sulfur battery, so that the shuttle effect of the polysulfide in electrolyte is inhibited, 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 structure2The preparation method of the C nano sheet comprises the following steps:
(1) will V2Stirring 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 suspension V2C, first powder;
(2) will V2C, 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 structure2C nano-sheet.
Further, V in step (2)2The mass ratio of the first powder to the sodium alginate is 50:1, the volume ratio of the deionized water to the ethylenediamine is 10:1, and the mass ratio is 200 to 200mgV2C the first powder needs to be added with 3mL of ethylenediamine.
Furthermore, the time of the hydrothermal reaction is 10-16 h.
V with filamentous structure prepared by the preparation method2C nano-sheet.
V having a filament structure as described above2Application of C nanosheet in lithium-sulfur battery, namely applying V2Mixing the C nanosheet and pure sulfur according to a ratio of 7:3, firstly preserving heat for 30min at 40 ℃, then preserving heat for 10h at 160 ℃ to carry sulfur to obtain a positive electrode material, uniformly mixing the obtained positive electrode material with acetylene black and PVDF according to a mass ratio of 7:2:1, adding N-methyl pyrrolidone to mix into slurry, coating the slurry on an aluminum foil, and drying to obtain the positive electrode plate of the lithium-sulfur battery. Preferably, V2The loading capacity of the C nano sheet on the aluminum foil is 2.3 mg/cm2The 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 structure2C nanosheet 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 structure2The C nanosheet is simple to operate, has low requirements on equipment and canRealizing industrialized production. V obtained thereby2The 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.
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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 invention2C, scanning electron microscope image of the nanosheet;
FIG. 2 shows a V with a filamentous structure according to example 2 of the present invention2C, scanning electron microscope image of the nanosheet;
FIG. 3 shows a V with a filamentous structure according to example 3 of the present invention2C, scanning electron microscope image of the nanosheet;
FIG. 4 shows a V having a filament-like structure according to comparative example 1 of the present invention2C, transmission electron microscope image of the nanosheet;
FIG. 5 shows a V of a filamentous structure provided in comparative example 2 of the present invention2C, transmission electron microscope image of the nanosheet;
FIG. 6 shows a V of a filamentous structure provided in comparative example 3 of the present invention2C, transmission electron microscope image of the nanosheet;
FIG. 7 shows a V of a filamentous structure provided in comparative example 4 of the present invention2C, transmission electron microscope image of the nanosheet;
FIG. 8 shows a V of a filamentous structure provided in comparative example 5 of the present invention2C, transmission electron microscope image of the nanosheet;
FIG. 9 shows V provided in example 1 of the present invention and comparative example 12A performance diagram of a lithium-sulfur battery made of C nanosheets;
FIG. 10 shows inventive example 1 and comparative exampleExample 1 provides V2And 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 clearer, the technical solutions in 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 not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a V with a filamentous structure2C nanosheet 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 structure2The C nanosheet is simple to operate, has low requirements on equipment, and can realize industrial production. V obtained thereby2The 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 structure2C nano sheet, its preparation method is as follows:
s1, 500mg of V is taken2Stirring AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly washing 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 V2C, first powder;
s2 at N2Under protective atmosphere, 200mg of lyophilized V was taken2Dispersing 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, and after the reaction is finished, carrying out hydrothermal reaction on the suspension for 12hCooling to room temperature, centrifuging, and vacuum drying at 60 deg.C for 24 hr to obtain V with filamentous structure2C nanosheet; the scanning electron micrograph is shown in FIG. 1, at adjacent V2A small amount of nanoribbons can be observed between the C layers.
Example 2
V with filiform structure2C nano sheet, its preparation method is as follows:
s1, 500mg of V is taken2Stirring AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly washing 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 V2C, first powder;
s2 at N2Under protective atmosphere, 200mg of lyophilized V was taken2Dispersing 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 carrying out vacuum drying at 60 ℃ for 24h to obtain the V with the filamentous structure2C nanosheet; as shown in fig. 2, it can be seen that various nanobelts are generated, which tightly weave discrete nanosheets together to form an interconnected 3D structure.
Example 3
V with filiform structure2C nano sheet, its preparation method is as follows:
s1, taking 500mg V2Stirring AlC powder and 20mL of hydrofluoric acid solution (49 wt%) for 55h at normal temperature, repeatedly washing 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 V2C, first powder;
s2. in N2Under protective atmosphere, 200mg of lyophilized V was taken2Dispersing 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 180 ℃ for 12h, cooling to room temperature after the reaction is finished, centrifuging, and carrying out vacuum drying at 60 ℃ for 24h to obtain the sodium alginate-based composite materialPrecipitating to black; the scanning electron micrograph is shown in FIG. 3, V2The C nanoplatelets almost disappear at high temperatures of 180 ℃, and instead are rich, inter-woven nanobelts and some discretely distributed nanoplatelets.
Comparative example 1
This comparative example provides a layered V2The 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 shown2The C nano-plate has no obvious morphological change compared with the C nano-plate, which means that the change of the morphology needs to overcome a certain reaction barrier.
Comparative example 2
This comparative example provides a layered V2C nano sheet, the preparation method is the same as that of example 1, except 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 seen2The edges and the surface of the C nano-sheets form a large number of nano-belts with the width less than 20 nm, and an interconnected 3D structure is formed.
Comparative example 3
This comparative example provides a layered V2C 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 seen2The C-nanoplatelets have become intertwined filamentous nanoribbons.
Comparative example 4
This comparative example provides a layered V2C 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 V2C, the surface of the nanosheet.
Comparative example 5
This comparative example provides a layered V2C nano sheet, the preparation method is the same as that of example 1, except that the hydrothermal time is prolonged to 30h, and the transmission electron microscope is shown in figures 8a and 8b, and the nano belt can be seenSome nanodots are also present.
Test example 1
V in examples 1 to 3 and comparative examples 1 to 5 was used2And C, observing and recording the structural shape under an electron microscope, wherein the recording result is shown in Table 1.
TABLE 1 layered filaments V2C nanosheet structure shape contrast
Figure DEST_PATH_IMAGE001
As can be seen from Table 1, V with different morphologies can be obtained by controlling the hydrothermal reaction time at the same hydrothermal temperature2C nanoplatelets, herein proposed a shear mechanism mediated by SA to form filamentous structures. Under the alkalescent environment (the function of the ethylenediamine), the SA is rich in functional groups, is a linear polysaccharide with rich carboxyl/hydroxyl, can be used as a reaction igniter in a beta-D mannuronic acid unit and an alpha-L guluronic acid unit, and is V2The delamination and fracture of the C nanosheets provide a powerful driver. V2Edge V atom and V of C surface2Extensive hydrogen bonding between C and SA can weaken the adjacent V2The 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 V2An exploration experiment of the influence of the C nanosheet morphology shows that nanobelts are gradually generated by continuous prolonging of the time from comparative example 1 to comparative example 3, but V can be found from comparative example 4 and comparative example 5 when the time is prolonged to 16h and then the time of hydrothermal reaction is prolonged2The nanoplatelets of C have been destroyed.
Test example 2
V with filamentous Structure prepared by example 12C nanosheet, and preparation of comparative example 1V without filament structure2The C nanosheets are respectively used as carriers of the positive electrode sulfur, applied to the lithium sulfur battery and tested for performance, and the test results are shown in table 2, wherein the manufacturing process of the lithium sulfur battery is as follows: v from example 12C nanosheet or layered V made in comparative example 12Mixing 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 for 30min at 40 ℃, and then reacting for 10h at 160 ℃ to carry out sulfur, thereby obtaining the cathode material. Preferably, said layered V2When the C nano sheet reacts with the pure sulfur, the temperature is increased to 40 ℃ from room temperature at the speed of 1-3 ℃/min, the temperature is kept at 40 ℃ for 30min, and then the temperature is increased to 160 ℃ at the speed of 3 ℃/min and the temperature is kept for 10 h.
Uniformly mixing the obtained positive electrode material with acetylene black and PVDF according to the mass ratio of 7:2:1, adding N-methyl pyrrolidone to mix into slurry, coating the slurry on an aluminum foil, and carrying sulfur-loaded V2The surface loading of the C nano sheet is 2.3 mg/cm2And standing in an oven at 50 ℃ for 720 min to obtain the positive plate. Lithium sheet (diameter 0.8 cm) as negative electrode, 1.0M DME/DOL of LiTFSI (volume ratio 1: 1) with 2.0 wt.% LiNO3As electrolyte, a battery is assembled in a glove box, and the charging and discharging voltage is 2.8V-1.6V (vs. Li/Li)+) 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
Figure DEST_PATH_IMAGE002
As can be seen from Table 2, V having a filamentous structure provided by the examples of the present invention2The 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 filamentous structures2The capacity of the C nano-sheet is much smaller, and is only 1050 mAh & g-1. As shown in fig. 10, and after 100 cycles at 0.5CThe capacity of example 1 was maintained at 820 mAh g-1In contrast, comparative example 1 had only 408 mAh g-1. Should be the electrolyte penetrate into V having a filamentous structure2In 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 (8)

1. V with filiform structure2The preparation method of the C nanosheet is characterized by comprising the following steps:
(1) will V2Stirring 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 V2C, first powder;
(2) will V2C, 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 structure2C nano-sheet.
2. V with filamentary structure according to claim 12The preparation method of the C nano-sheet is characterized in that V in the step (2)2And C, the mass ratio of the first powder to the sodium alginate is 50:1, and the volume ratio of the deionized water to the ethylenediamine is 10: 1.
3. V with filamentary structure according to claim 12The preparation method of the C nanosheet is characterized in that the hydrothermal reaction time is 10-16 h.
4. V having a filamentous structure obtained by the production method according to any one of claims 1 to 32C nano-sheet.
5. V with filamentous structure according to claim 42The application of the C nano sheet in the lithium-sulfur battery is characterized in that V is added2And mixing the C nanosheet and sulfur according to a ratio 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 a mass ratio of 7:2:1, adding N-methyl pyrrolidone to mix into slurry, coating the slurry on an aluminum foil, and drying to obtain the positive electrode plate of the lithium-sulfur battery.
6. Use according to claim 5, characterized in that V2The loading capacity of the C nano sheet on the aluminum foil is 2.3 mg/cm2The drying refers to drying at 50 ℃ for 720 min.
7. The use according to claim 5, wherein the sulfur loading is carried out by first holding at 40 ℃ for 30min and then holding at 160 ℃ for 10 h.
8. The use according to any one of claims 5 to 7, wherein the battery is assembled in a glove box using a lithium plate as the negative electrode and a 1.0M LiTFSI DME/DOL solution as the electrolyte.
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