CN110921704A - Vanadium disulfide @ carbon paper nano material, preparation method thereof and magnesium-lithium double-ion battery - Google Patents
Vanadium disulfide @ carbon paper nano material, preparation method thereof and magnesium-lithium double-ion battery Download PDFInfo
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- C01G31/00—Compounds of vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention provides a vanadium disulfide @ carbon paper nano material, a preparation method thereof and a magnesium-lithium double-ion battery, and belongs to the technical field of magnesium-lithium double-ion batteries. The invention provides a preparation method of a vanadium disulfide @ carbon paper nano material, which comprises the following steps: n-octylamine and NH4VO3Mixing with thioacetamide to obtain a mixed solution; carrying out solvothermal reaction on the mixed solution and carbon paper to obtain the vanadium disulfide @ carbon paper nano material. According to the invention, octylamine small molecules are embedded into vanadium disulfide by a solvothermal method, so that the distance between van der Waals force layers is increased, magnesium ions and lithium ions are jointly embedded and de-embedded, the battery capacity is improved, and as the microstructure becomes open, the ion migration path is also reduced, and the rate capability is increased.
Description
Technical Field
The invention relates to the technical field of magnesium-lithium double-ion batteries, in particular to a vanadium disulfide @ carbon paper nano material and a preparation method thereof, and a magnesium-lithium double-ion battery.
Background
As a commercialized metal ion battery, a lithium ion battery has advantages of high operating voltage, large energy density, and long cycle life. However, the safety problem caused by the growth of the lithium metal dendrite, the higher cost, the limited practical energy density and other problems restrict the further development of the lithium ion battery. The new magnesium ion battery has many advantages complementary to the lithium ion battery, but there are some factors that limit its development. The problem is particularly pronounced in many electrode materials, such as MoS, where one of the two positively charged magnesium ions is strongly polarized, resulting in slow diffusion kinetics of the magnesium ions in the positive electrode material2，NbS2And V2O5And the like. In order to solve this problem, the above-mentioned problem can be avoided by constructing a magnesium-lithium bi-ion battery by introducing lithium ions into a magnesium-ion electrolyte, because the positive electrode is mainly dominated by the rapid reaction of lithium ions after constructing the bi-ion battery, while the negative electrode is still deposited/exfoliated by magnesium ions. The magnesium-lithium double-ion system can be said to combine the safety and low cost of magnesium and the rapid reaction kinetics of lithium ions, and becomes a magnesium-based battery with great development prospect.
Currently, many electrode materials suitable for electrochemical windows of lithium ion batteries have been successfully applied to magnesium-lithium bi-ion batteries, such as MoS2、TiS2、VO2、LiFePO4However, these materials support only the intercalation/deintercalation of lithium ions, and thus have a problem of poor battery capacity and rate performance.
Disclosure of Invention
In view of the above, the invention aims to provide a vanadium disulfide @ carbon paper nanomaterial, a preparation method thereof and a magnesium-lithium dual-ion battery. According to the preparation method provided by the invention, n-octylamine molecules are embedded in advance, and the vanadium disulfide nanosheets are subjected to layer expanding modification, so that the ion migration path is favorably shortened, and the capacity and the rate capability of the battery are greatly improved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a vanadium disulfide @ carbon paper nano material, which comprises the following steps:
n-octylamine and NH4VO3Mixing with thioacetamide to obtain a mixed solution;
and carrying out solvothermal reaction on the mixed solution and carbon paper to obtain the vanadium disulfide @ carbon paper nano material.
Preferably, the n-octylamine, NH4VO3And the dosage ratio of thioacetamide is 12-15 mL: 0.081-0.082 g: 0.262 to 0.263 g.
Preferably, the carbon paper has a diameter of 16 mm.
Preferably, the temperature of the solvothermal reaction is 160-170 ℃ and the time is 20-24 h.
Preferably, after the solvothermal reaction, the obtained solvothermal reaction product is alternately cleaned for 4-6 times by using deionized water and ethanol, and then is dried for 10-12 hours in vacuum at the temperature of 60-80 ℃.
The invention also provides the vanadium disulfide @ carbon paper nano material prepared by the preparation method in the technical scheme, the morphology of the vanadium disulfide @ carbon paper nano material is a three-micro open structure self-assembled by two-dimensional vanadium disulfide nanosheets, n-octylamine molecules exist between layers (001) of the vanadium disulfide nanosheets, and the interlayer spacing of the layers (001) is 1.0 +/-0.02 nm.
Preferably, the percentage of the n-octylamine molecules embedded by mass is 16 ± 0.5%.
Preferably, the loading amount of the vanadium disulfide nanosheets on the carbon paper with the diameter of 16mm is 1.2-2.4 mg.
The invention also provides a magnesium-lithium double-ion battery, which takes magnesium foil as an anode, takes a positive plate coated with the vanadium disulfide @ carbon paper nano material as a positive electrode material in the technical scheme as a cathode, does not contain a binder, takes Whatman as a diaphragm, and takes LiCl and anhydrous A as materialslCl3And the product synthesized with PhMgCl in tetrahydrofuran is the electrolyte.
Preferably, the mass density of the vanadium disulfide @ carbon paper nano material on the positive plate is 0.6-1.2 g-cm-2。
The invention provides a preparation method of a vanadium disulfide @ carbon paper nano material, which comprises the following steps: n-octylamine and NH4VO3Mixing with thioacetamide to obtain a mixed solution; and carrying out solvothermal reaction on the mixed solution and carbon paper to obtain the vanadium disulfide @ carbon paper nano material.
According to the invention, octylamine small molecules are embedded into vanadium disulfide by a solvothermal method, so that the distance between van der Waals force layers is increased, magnesium ions and lithium ions are jointly embedded and de-embedded, the battery capacity is improved, and as the microstructure becomes open, the ion migration path is also reduced, and the rate capability is increased. The invention prepares the binderless, interlayer expanded, vanadium disulfide @ carbon paper (E-VS)2@ C) nano material is used as a novel positive electrode material of the magnesium-lithium double-ion battery, and the following advantages are given to the application of the magnesium-lithium double-ion battery through the unique structural characteristics of the electrode material: (1) the process flow of battery assembly is simplified. Generally, the positive electrode material needs to be mixed with an additive binder and a conductive carbon material according to a certain proportion, and the complete positive electrode material can be prepared through continuous multi-step processes of pulping, coating, drying and the like, and the existence of the binder increases the possibility of side reactions of the battery. E-VS prepared by the invention2The @ C does not need an adhesive, the process is greatly simplified due to the characteristic of no adhesive, and unnecessary side reactions are avoided; (2) the battery capacity is obviously improved. Vanadium disulfide is embedded into small molecule octylamine, so that the distance between van der waals force layers is greatly increased, and more ions can be accommodated, and the capacity is increased. At 100mA · g-1The current density can be kept as high as 255.0 mAh.g-1A specific capacity of the left and right; (3) the multiplying power cycling performance is improved. The expanded vanadium disulfide can better adapt to the repeated charge-discharge process, the damage of the ion intercalation and deintercalation process to the electrode material is reduced, and the nano-sheet open structure is favorable for shortening the migration path of ionsThe contact area with the electrolyte is increased, so that the multiplying power cycle performance of the battery is improved. At 5 A.g-1Still maintains 136.0mAh g at high current density-1Specific capacity of (a); (4) binderless E-VS as compared to the positive electrode materials of many magnesium-lithium dual ion batteries2The @ C nano material as a novel positive electrode material of the magnesium-lithium double-ion battery shows a higher average voltage of about 1.2V.
Drawings
FIG. 1 is an open circuit voltage test chart;
FIG. 2 shows 100mA · g-1Constant current cyclic charge-discharge specific volume and coulombic efficiency curve under current density;
FIG. 3 is a graph of the first three constant current charge and discharge curves of a Mg-Li bi-ion battery;
FIG. 4 is a graph of a rate capability test;
FIG. 5 is a cyclic voltammetry test curve;
FIG. 6 shows E-VS2SEM image of @ C, where (a) and (b) are respectively E-VS2@ C SEM images at different magnifications;
FIG. 7 shows E-VS2TEM image of @ C, where (a), (b) and (C) are E-VS, respectively2TEM images at different magnifications @ C;
FIG. 8 shows E-VS2V, S, C and N element distribution images in @ C;
FIG. 9 shows E-VS2@ C and VS2XRD pattern of (a).
Detailed Description
The invention provides a vanadium disulfide @ carbon paper nano material (E-VS)2@ C), comprising the following steps:
n-octylamine and NH4VO3Mixing with thioacetamide to obtain a mixed solution;
and carrying out solvothermal reaction on the mixed solution and carbon paper to obtain the vanadium disulfide @ carbon paper nano material.
In the invention, the n-octylamine and NH4VO3And the preferable dosage ratio of thioacetamide is 12-15 mL: 0.081-0.082 g: 0.262 to 0.263 g. The invention utilizes ZhengxinThe amine carries out layer expansion modification on the vanadium disulfide, so that the vanadium disulfide layers are expanded, the morphological structure of the vanadium disulfide layers is optimized and more open, the ion migration path is favorably shortened, the ion embedding and de-embedding are favorably realized, and the capacity and the rate capability of the battery are greatly improved.
In the present invention, the carbon paper preferably has a diameter of 16 mm.
In the invention, the temperature of the solvothermal reaction is preferably 160-170 ℃, and the time is preferably 20-24 h. In the present invention, the solvothermal reaction is preferably carried out in an autoclave with a 35mL sealed polytetrafluoroethylene liner.
In the invention, after the solvothermal reaction, the method preferably further comprises the steps of alternately cleaning the obtained solvothermal reaction product with deionized water and ethanol for 4-6 times, and then drying the product in vacuum at the temperature of 60-80 ℃ for 10-12 hours.
The invention also provides the vanadium disulfide @ carbon paper nano material prepared by the preparation method in the technical scheme, the morphology of the vanadium disulfide @ carbon paper nano material is a three-micro open structure self-assembled by two-dimensional vanadium disulfide nanosheets, n-octylamine molecules exist between layers (001) of the vanadium disulfide nanosheets, and the interlayer spacing of the layers (001) is 1.0 +/-0.02 nm.
In the present invention, the percentage of the n-octylamine molecules inserted by mass is preferably 16 ± 0.5%.
In the invention, the preferable load capacity of the vanadium disulfide nanosheet on the carbon paper with the diameter of 16mm is 1.2-2.4 mg.
The invention also provides a magnesium-lithium double-ion battery, which takes a magnesium foil as an anode, takes a positive plate coated with the vanadium disulfide @ carbon paper nano material as a positive electrode material in the technical scheme as a cathode, does not contain a binder, takes Whatman (GF/F) as a diaphragm, and takes LiCl and anhydrous AlCl as materials3And the product synthesized with PhMgCl in tetrahydrofuran is the electrolyte.
In the present invention, the thickness of the magnesium foil is preferably 0.2mm, and the purity is preferably 99.99%.
In the invention, the mass density of the vanadium disulfide @ carbon paper nano material on the positive plate is preferably 0.6-1.2 g-cm-2。
The preparation method of the magnesium-lithium double-ion battery is not particularly limited, and the magnesium-lithium double-ion battery can be prepared by adopting a preparation method well known to a person skilled in the art.
In order to further illustrate the invention, the vanadium disulfide @ carbon paper nanomaterial and the preparation method thereof and the magnesium-lithium dual-ion battery provided by the invention are described in detail by combining the examples below, but the examples should not be construed as limiting the scope of the invention.
Example 1
Step 1: sample preparation
Solvothermal method for synthesizing E-VS2@ C: 12mL of n-octylamine was weighed into 35mL of Teflon liner. 0.081g of NH is weighed4VO3And 0.262g of thioacetamide are sequentially added into the polytetrafluoroethylene lining containing the n-octylamine, and after the mixture is stirred for 1 hour, a piece of carbon paper with the diameter of 16mm is added into the mixture. Then sealing the polytetrafluoroethylene lining in a high-pressure reaction kettle, and reacting for 20 hours at 160 ℃. After the reaction is finished, taking out the carbon paper, alternately cleaning the carbon paper for 4 times by using deionized water and ethanol, and drying the carbon paper for 10 hours in vacuum at the temperature of 60 ℃ to obtain the E-VS2@C，VS2The loading amount on the carbon paper ranges from 1.2 mg to 2.4mg, and the octylamine embedding mass percentage is 16 +/-0.5%.
Step 2: battery system
Preparation of positive pole piece
Will E-VS2@ C was used as a positive electrode for a battery as it is, and the mass density of the active material was 0.6 g-cm-2。
Assembly of CR2025 button cell
Using magnesium foil as anode, the thickness of the magnesium foil is 0.2mm, the purity is 99.99%, and E-VS2@ C is a positive electrode material, and Whatman (GF/F) is a separator. With LiCl and anhydrous AlCl3And PhMgCl in tetrahydrofuran and as an electrolyte. The assembly of each part of the button cell is completed according to the assembly sequence, and the packaging of the cell is completed on a sealing machine.
And step 3: electrochemical testing
1) Open circuit voltage testing
Fig. 1 is a test chart of open circuit voltage, which shows that the open circuit voltage is about 1.74V, and two batteries can be connected in series to light a 3V led.
2) Constant current cycling test
Constant current cycling test was performed using a LAND CT2001A battery test system with a current density of 100mA g-1The voltage range is set to be 0.25-2V.
FIG. 2 shows 100mA · g-1Constant current cyclic charge-discharge specific volume and coulombic efficiency curve under current density. As can be seen, the specific first discharge capacity is 309mAh g-1The corresponding coulombic efficiency was 87.4%. The constant-current circulation process is stable, and after 100 times of circulation, the discharge specific capacity can still maintain 256mAh g-1The coulombic efficiency was 100%, and the cycle retention rate relative to the second turn was 94.8%. To illustrate, E-VS without adhesive2The @ C nano material as a novel positive material of the magnesium-lithium double-ion battery shows high specific capacity, excellent cycle stability and cycle capacity retention rate.
Fig. 3 is a graph of the first three constant current charge and discharge curves of a magnesium-lithium bi-ion battery. As can be seen from FIG. 3, there is no adhesive E-VS2The @ C nano material is used as a novel positive electrode material of the magnesium-lithium double-ion battery, has several charging and discharging voltage slopes, and shows a multi-step ion intercalation and deintercalation process. The discharge voltage ramp ranges from 1.6V to 1.75V, from 1.25V to 1.50V and from 1.00V to 1.25V, and the charge voltage ramp ranges from 1.25V to 1.80V.
3) Rate capability test
The rate capability test was performed on a LAND CT2001A battery test instrument. As shown in FIG. 4, the current density was varied from 100mA · g in ten cycles-1Increased to 5000mA g-1It can be seen that the capacity is maintained at 5000mA · g with a large amount of current density increasing and decreasing-1Still maintain 136mAh g under high current density-1And at a current density of 100mA g again-1263 mAh.g. still visible-1(98.1%) specific capacity, indicating E-VS without binder2@ C nanomaterial as magnesium lithiumThe novel positive electrode material of the dual-ion battery shows better rate performance.
4) Cyclic voltammetry test
Cyclic voltammetry tests were performed on a Gamry Interface 1000. The scanning rate was 0.2 mV.s-1The scan voltage range is 0.25-2V.
The cyclic voltammetry test curve is shown in FIG. 5, from which it can be seen that there is no binder E-VS2The @ C nano material is used as a novel positive material of the magnesium-lithium double-ion battery, and shows cathode peak current at 1.6V, 1.28V, 1.0V and 0.7V respectively, and anode peak current at 1.3V and 1.75V respectively, and the range of the @ C nano material is similar to that of a charging and discharging voltage slope.
Step 4 topography characterization
1) Scanning Electron microscope testing (SEM)
FIGS. 6(a) and (b) are E-VS, respectively2In SEM images of @ C under different magnifications, the appearance of the material is a three-micro open structure self-assembled by two-dimensional vanadium disulfide nanosheets. The nano self-assembly particle size is about 1 mu m, and the thickness of the nano sheet is about 20 nm. The three-dimensional open structure is beneficial to shortening the ion transmission path, thereby improving the electrochemical performance.
2) Transmission electron microscope Test (TEM)
FIGS. 7(a), (b) and (c) are E-VS, respectively2In TEM images of @ C at different magnifications, it can be seen from FIGS. 7(a) and (b) that the expanded vanadium disulfide exhibits a clear three-dimensional hierarchical open structure. Fig. 7(c) is a high-resolution transmission electron micrograph showing that the lattice spacing is 1.0nm as seen by the lattice fringes and the van der waals force interplanar spacing after layer expansion, indicating that the interlayer spacing of vanadium disulfide was successfully expanded from 0.57nm to 1.0 nm.
3) Auger electron spectroscopy test (EDS)
FIG. 8 shows E-VS2The element distribution image of V, S, C and N in @ C, as can be seen from FIG. 8, V and S are uniformly distributed on the nanosheet self-assembled structure. In addition, the uniform distribution of the N element in the element distribution also indicates intercalation of the octylamine molecules.
3) X-ray diffraction (XRD)
FIG. 9 shows E-VS2@ C and VS2XRD pattern of (D), as can be seen in FIG. 9, E-VS2And E-VS2The XRD pattern of @ C showed diffraction peaks at 8.7 °, 18.0 ° and 56.8 ° at 2 θ, which were shifted toward low angles with respect to the unexpanded vanadium disulfide layer, indicating that the interlayer spacing was expanded, and the (001) interlayer spacing after expansion was 1.0 ± 0.02 nm. This indicates that the octylamine molecule exists between (001) layers to extend the interlayer spacing.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A preparation method of a vanadium disulfide @ carbon paper nano material is characterized by comprising the following steps:
n-octylamine and NH4VO3Mixing with thioacetamide to obtain a mixed solution;
and carrying out solvothermal reaction on the mixed solution and carbon paper to obtain the vanadium disulfide @ carbon paper nano material.
2. The method according to claim 1, wherein the n-octylamine or NH is used as a catalyst4VO3And the dosage ratio of thioacetamide is 12-15 mL: 0.081-0.082 g: 0.262 to 0.263 g.
3. A production method according to claim 1 or 2, characterized in that the carbon paper has a diameter of 16 mm.
4. The preparation method according to claim 1, wherein the temperature of the solvothermal reaction is 160-170 ℃ and the time is 20-24 h.
5. The preparation method according to claim 1, wherein after the solvothermal reaction, the obtained solvothermal reaction product is alternately cleaned with deionized water and ethanol for 4-6 times, and then dried under vacuum at 60-80 ℃ for 10-12 h.
6. The vanadium disulfide @ carbon paper nanomaterial prepared by the preparation method of any one of claims 1 to 5, wherein the morphology of the vanadium disulfide @ carbon paper nanomaterial is a three-micron open structure self-assembled by two-dimensional vanadium disulfide nanosheets, n-octylamine molecules exist between layers (001) of the vanadium disulfide nanosheets, and the interlayer spacing of the layers (001) is 1.0 +/-0.02 nm.
7. The vanadium disulfide @ carbon paper nanomaterial as claimed in claim 6, wherein the n-octylamine molecules are embedded in a mass percentage of 16 ± 0.5%.
8. The vanadium disulfide @ carbon paper nanomaterial according to claim 6 or 7, wherein the loading amount of vanadium disulfide nanosheets on carbon paper with a diameter of 16mm is 1.2-2.4 mg.
9. A magnesium-lithium double-ion battery is characterized in that a magnesium foil is used as an anode, a positive plate coated with the vanadium disulfide @ carbon paper nano material as claimed in any one of claims 6 to 8 is used as a cathode, no binder is contained, Whatman is used as a diaphragm, LiCl and anhydrous AlCl are used3And the product synthesized with PhMgCl in tetrahydrofuran is the electrolyte.
10. The magnesium-lithium bi-ion battery of claim 9, wherein the mass density of the vanadium disulfide @ carbon paper nanomaterial on the positive electrode sheet is 0.6-1.2 g-cm-2。
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| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
| CN113036103A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery |
| CN114156447A (en) * | 2021-11-17 | 2022-03-08 | 南京来璋新材料科技有限公司 | Sandwich structure composite material for magnesium ion battery anode and preparation method thereof |
| CN114843476A (en) * | 2022-05-20 | 2022-08-02 | 重庆大学 | V-shaped groove 3 S 4 Preparation method and application of @ C/G composite electrode material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
| CN113036103A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery |
| CN114156447A (en) * | 2021-11-17 | 2022-03-08 | 南京来璋新材料科技有限公司 | Sandwich structure composite material for magnesium ion battery anode and preparation method thereof |
| CN114843476A (en) * | 2022-05-20 | 2022-08-02 | 重庆大学 | V-shaped groove 3 S 4 Preparation method and application of @ C/G composite electrode material |
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