CN109830659B - Te-doped MXene material and preparation method thereof - Google Patents
Te-doped MXene material and preparation method thereof Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a Te doped MXene material and a preparation method thereof, and the preparation method comprises the following steps: (1) mixing MXene and Te sources according to the mass ratio of 1: 0.01-1, adding the mixture into a dispersing agent to prepare a dispersing solution with the concentration of 1-100mg/ml, and then stirring for 1-5 hours; (2) heating the dispersion liquid to 100-220 ℃, reacting for 10-24h, and then cooling to room temperature; (3) cleaning the product obtained in the step (2) by using a cleaning agent, and then centrifuging; (4) and (4) drying the centrifugal product obtained in the step (3) in vacuum to obtain the Te doped MXene material. Compared with an undoped MXene material, the composite material prepared by the invention can increase the MXene interlayer spacing by doping Te, generate more electrochemical active sites, is beneficial to ion diffusion, and improves the electrode conductivity, potassium storage capacity and cycling stability.
Description
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a Te-doped MXene material and a preparation method thereof.
Background
MXene materials are a new two-dimensional series of metal carbides and carbonitrides, where M is a transition metal, a is group IIIA or group IVA and X is C or N. Under the action of hydrofluoric acid, A atoms are removed by corrosion, so that a nano flaky material which contains functional groups of hydroxyl, oxygen and fluorine and has ultrahigh specific surface area is formed. The material has the advantages that the material has more active sites and contact area with electrolyte due to the ultra-high specific surface area, reaction kinetics are reduced, and MXene has excellent hydrophilic surface and good conductivity due to various chemical components and rich functional groups, so that the material has great application potential in the field of energy storage.
MXene has shown good electrochemical performance in energy storage devices due to unique structure and physicochemical properties, and Li, Na, K and Ca in Ti are obtained by calculation of Shenoy and the like3C2The capacitances above were 447.8, 351.8, 191.8 and 319.8mA/g, respectively, and MXene, used by Simon et al as a sodium ion capacitor, achieved a capacitance of 100F/g at 0.2 mV/s. Nevertheless, when pure MXene is used as an electrode material, some electrochemical properties are still unsatisfactory. Such as: poor conductivity, low mass capacity, etc., and performance improvements are needed. Chemical doping is a common modification means, and the defect concentration and the electron concentration are improved by introducing new chemical elements and distorting crystal lattices. Although a technology of doping MXene with sulfur has been proposed, on one hand, hydrogen sulfide is used as a sulfur source, so that the toxicity is high, the pollution is serious, and the subsequent treatment is difficult; on the other hand, the radius of S atom is smaller than that of tellurium atom, resulting in less lattice distortion and limited improvement of performance. After the tellurium is doped into MXene, the lattice distortion is large, and the defect concentration is highMore, wider interlamellar spacing, richer active sites and wider application prospect.
In the existing battery industry, the method or the process steps for preparing the battery are more, so the cost is easily increased, and the performance is reduced if some process steps are simply omitted. Therefore, the Te-doped MXene material and the battery thereof which are low in cost, safer and more environment-friendly and prepared by the simple method have important practical significance.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a Te-doped MXene material. The invention also aims to provide a preparation method of the Te-doped MXene material. Further, the invention provides application of the Te doped MXene material, wherein the Te doped MXene material is used as a potassium ion battery negative electrode.
The invention adopts the following technical scheme:
a preparation method of Te doped MXene material belongs to a solvothermal method and comprises the following steps:
(1) mixing MXene and Te sources according to the mass ratio of 1: (0.01-1), optionally 1: (0.1-0.9), optionally 1: (0.2-0.8), optionally 1: (0.4-0.6) adding the dispersion into a dispersing agent to prepare a dispersion with the concentration of 1-100mg/ml, optionally 10-90mg/ml, optionally 20-80mg/ml, optionally 40-60mg/ml, and then stirring for 1-5 hours, optionally 1, 2, 3, 4 and 5 hours;
(2) heating the dispersion to 100-220 ℃ (for example, sealing the dispersion in a reaction kettle and then placing the dispersion in an oven for reaction), reacting for 10-24h, and then cooling to room temperature;
(3) cleaning the product obtained in the step (2) by using a cleaning agent, and then centrifuging;
(4) and (4) drying the centrifugal product obtained in the step (3) in vacuum (for example, in a vacuum drying oven) to obtain the Te doped MXene material.
Further, the Te source is at least one of biphenyl ditelluride, sodium tellurite, and tellurium powder (particle size is 80-120 mesh, for example, 100 mesh).
Further, MXene is Ti3C2Tx、Ti2CTx、V3C2Tx、V3N2Tx、V2CTxOptionally Ti3N2TxOptionally V3C2TxOptionally V3N2TxPreferably, the mass ratio is 4-9: 1 of Ti3C2TxAnd V3C2TxOptionally Ti3C2Tx、V3N2TxAnd V3C2Tx(e.g., mass ratio of 4-9: 1: 1), TxIs a surface functional group-O, -F or-OH.
Further, the dispersant is at least one of N, N-dimethylformamide and ethanol.
Further, the cleaning agent is at least one of water (preferably ultrapure water) and ethanol. The product obtained in step (2) is preferably thoroughly washed with ultrapure water and anhydrous ethanol, and may be alternately washed with ultrapure water and anhydrous ethanol 2 to 15 times, preferably 3 to 8 times.
Further, the Te doping amount in the Te doping MXene material is 1-20 wt%, such as 3-18 wt%, 5-15 wt%, 6-12 wt% and 7-8 wt%.
Further, in the step (2), the temperature of the dispersion liquid in the reaction kettle is raised to 110-.
Further, the rotation speed used in the centrifugation in the step (3) is 4000-.
Further, the temperature of vacuum drying in the step (4) is 50-70 ℃, preferably 60 ℃, and the drying time is 8-12 hours, and 8, 9, 10, 11 and 12 hours can be selected. The vacuum does not exceed 135Pa, for example does not exceed 133, 130, 120, 110, 100, 90 Pa.
A Te-doped MXene material prepared by the preparation method of the Te-doped MXene material.
The application of the Te-doped MXene material is to use the Te-doped MXene material in a potassium ion battery negative electrode.
The invention has the beneficial effects that:
(1) compared with an undoped MXene material, the prepared composite material can increase the MXene interlayer spacing by doping Te, generates more electrochemical active sites, is beneficial to ion diffusion, and improves the electrode conductivity, potassium storage capacity and cycling stability;
(2) the material of the invention has simple preparation method and low cost, and is suitable for large-scale application.
Drawings
Fig. 1 is a scanning electron microscope image of undoped MXene material in comparative example 1;
FIG. 2 is a scanning electron microscope image of the Te doped MXene material in example 1;
FIG. 3 is a C-V plot of undoped MXene material of comparative example 1;
fig. 4 is a C-V plot of Te doped MXene material as measured in example 1.
Detailed Description
For better explanation of the present invention, the following specific examples are further illustrated, but the present invention is not limited to the specific examples.
Example 1
A preparation method of a Te-doped MXene material comprises the following steps:
(1) taking 50mg MXene (Ti)3C2Tx) And 0.5mg of biphenylditellurium were added to DMF to prepare a 1mg/ml DMF dispersion, which was magnetically stirred for 1 hour;
(2) transferring the dispersion liquid obtained in the step (1) to a reaction kettle with the capacity of 100ml, sealing, placing in an oven, preserving heat for 10 hours at 100 ℃, and cooling to room temperature;
(3) washing the product obtained in the step (2) with ultrapure water and absolute ethyl alcohol for 3 times respectively, and centrifuging for 5 minutes by a centrifuge under the condition of 5000 r/min;
(4) and (4) drying the centrifugal product obtained in the step (3) in a vacuum drying oven at the drying temperature of 60 ℃ for 8 hours.
Mixing the Te-doped MXene material, a polyvinylidene fluoride binder and carbon black according to the mass ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, uniformly stirring to form slurry, coating the slurry on a current collector, and performing vacuum drying and slicing to obtain the potassium ion battery negative plate.
The reversible capacity of the doped MXene material (used as a potassium ion battery cathode) in the embodiment after 100 cycles is 302mAh/g under the current density of 100mA/g, which is 3.1 times of that of the undoped MXene potassium ion battery cathode (97.2mAh/g) in FIG. 3, and the doped MXene material in the embodiment has very stable charge-discharge cycle performance.
Example 2
A preparation method of a Te-doped MXene material comprises the following steps:
(1) 1000mg of MXene (Ti) was taken2CTx) And 500mg of biphenylditellurium were added to DMF to prepare a 50mg/ml DMF dispersion, which was magnetically stirred for 3 hours;
(2) transferring the dispersion liquid obtained in the step (1) to a reaction kettle with the capacity of 50ml, sealing, placing in an oven, preserving heat for 15 hours at 150 ℃, and cooling to room temperature;
(3) washing the product obtained in the step (2) with ultrapure water and absolute ethyl alcohol for 3 times respectively, and centrifuging for 5 minutes by a centrifuge under the condition of 5000 r/min;
(4) and (4) drying the centrifugal product obtained in the step (3) in a vacuum drying oven at the drying temperature of 60 ℃ for 10 hours.
Mixing the Te-doped MXene material, a polyvinylidene fluoride binder and carbon black according to the mass ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, uniformly stirring to form slurry, coating the slurry on a current collector, and performing vacuum drying and slicing to obtain the potassium ion battery negative plate.
The reversible capacity of the doped MXene material (used as a potassium ion battery cathode) in the embodiment after 100 cycles is 321mAh/g under the current density of 100mA/g, which is 3.3 times of that of the undoped MXene potassium ion battery cathode (97.2mAh/g), and the doped MXene material in the embodiment has very stable charge-discharge cycle performance.
Example 3
A preparation method of a Te-doped MXene material comprises the following steps:
(1) 2000mg of MXene (b)Ti2CTx) And 2000mg of biphenylditellurium were added to DMF to prepare 100mg/ml DMF dispersion, which was magnetically stirred for 5 hours;
(2) transferring the dispersion liquid obtained in the step (1) to a reaction kettle with the capacity of 50ml, sealing, placing in an oven, preserving heat for 24 hours at 220 ℃, and cooling to room temperature;
(3) washing the product obtained in the step (2) with ultrapure water and absolute ethyl alcohol for 3 times respectively, and centrifuging for 5 minutes by a centrifuge under the condition of 5000 r/min;
(4) and (4) drying the centrifugal product obtained in the step (3) in a vacuum drying oven at the drying temperature of 60 ℃ for 12 hours.
Mixing the Te-doped MXene material, a polyvinylidene fluoride binder and carbon black according to the mass ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, uniformly stirring to form slurry, coating the slurry on a current collector, and performing vacuum drying and slicing to obtain the potassium ion battery negative plate.
The reversible capacity of the doped MXene material (used as a potassium ion battery cathode) in the embodiment after 100 cycles is 289mAh/g which is 3.0 times of that of the undoped MXene potassium ion battery cathode (97.2mAh/g) under the current density of 100mA/g, and the doped MXene material in the embodiment has very stable charge-discharge cycle performance.
Example 4
A preparation method of a Te-doped MXene material comprises the following steps:
(1) 1000mg of MXene (800mg of Ti) was taken2CTxAnd 200mg V2CTx) And 500mg of biphenylditellurium were added to DMF to prepare a 50mg/ml DMF dispersion, which was magnetically stirred for 3 hours;
(2) transferring the dispersion liquid obtained in the step (1) to a reaction kettle with the capacity of 50ml, sealing, placing in an oven, preserving heat for 10 hours at 110 ℃, and cooling to room temperature;
(3) washing the product obtained in the step (2) with ultrapure water and absolute ethyl alcohol for 3 times respectively, and centrifuging for 5 minutes by a centrifuge under the condition of 5000 r/min;
(4) and (4) drying the centrifugal product obtained in the step (3) in a vacuum drying oven at the drying temperature of 60 ℃ for 8 hours.
Mixing the Te-doped MXene material, a polyvinylidene fluoride binder and carbon black according to the mass ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, uniformly stirring to form slurry, coating the slurry on a current collector, and performing vacuum drying and slicing to obtain the potassium ion battery negative plate.
The reversible capacity of the doped MXene material (used as a potassium ion battery cathode) in the embodiment after 100 cycles is 331mAh/g under the current density of 100mA/g, which is 3.4 times of that of the undoped MXene potassium ion battery cathode (97.2mAh/g), and the doped MXene material in the embodiment has very stable charge-discharge cycle performance.
Example 5
A preparation method of a Te-doped MXene material comprises the following steps:
(1) 1000mg of MXene (V) was taken3N2Tx) And 400mg of sodium tellurite are added into DMF to prepare 50mg/ml DMF dispersion liquid, and the mixture is stirred for 3 hours by magnetic force;
(2) transferring the dispersion liquid obtained in the step (1) to a reaction kettle with the capacity of 50ml, sealing, placing in an oven, preserving heat at 120 ℃ for 11 hours, and cooling to room temperature;
(3) washing the product obtained in the step (2) with ultrapure water and absolute ethyl alcohol for 3 times respectively, and centrifuging for 5 minutes by a centrifuge under the condition of 5000 r/min;
(4) and (4) drying the centrifugal product obtained in the step (3) in a vacuum drying oven at the drying temperature of 60 ℃ for 9 hours.
Mixing the Te-doped MXene material, a polyvinylidene fluoride binder and carbon black according to the mass ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, uniformly stirring to form slurry, coating the slurry on a current collector, and performing vacuum drying and slicing to obtain the potassium ion battery negative plate.
The reversible capacity of the doped MXene material (used as a potassium ion battery cathode) in the embodiment after 100 cycles is 347mAh/g under the current density of 100mA/g, which is 3.6 times of that of an undoped MXene potassium ion battery cathode (97.2mAh/g), and the doped MXene material in the embodiment has very stable charge-discharge cycle performance.
Comparative example 1: MXene was undoped.
Table 1: performance testing
The above description is only exemplary of the present invention and is not intended to limit the scope of the present invention, which is defined by the claims appended hereto, as well as the appended claims.
Claims (6)
1. A preparation method of a Te doped MXene potassium ion battery negative electrode material is characterized by comprising the following steps:
(1) mixing MXene and Te sources according to the mass ratio of 1: 0.01-1, adding the mixture into a dispersing agent to prepare a dispersing solution with the concentration of 1-100mg/ml, and then stirring for 1-5 hours;
(2) transferring the dispersion liquid into a reaction kettle, heating to the temperature of 100 ℃ and 220 ℃, reacting for 10-24h, and then cooling to the room temperature;
(3) cleaning the product obtained in the step (2) by using a cleaning agent, and then centrifuging;
(4) vacuum drying the centrifugal product obtained in the step (3) to obtain the Te doped MXene potassium ion battery negative electrode material;
the Te source is at least one of biphenyl ditelluride and sodium tellurite;
the MXene is Ti2CTx、V3N2Tx 、V2CTxWherein T isxIs a surface functional group-O, -F or-OH;
the doping amount of Te in the Te-doped MXene potassium ion battery negative electrode material is 3.6-5.0 wt%;
the dispersant is at least one of N, N-dimethylformamide and ethanol; the cleaning agent is at least one of water and ethanol.
2. The method for preparing the Te-doped MXene material as claimed in claim 1, wherein the temperature of the dispersion liquid in the step (2) is raised to 110-200 ℃ in a reaction kettle, and the reaction lasts for 10-15 h.
3. The method for preparing the cathode material of the Te doped MXene potassium ion battery as claimed in claim 1, wherein the rotation speed for centrifugation in step (3) is 4000-6000r/min and centrifugation is 5-10 min.
4. The preparation method of the Te doped MXene potassium ion battery negative electrode material as claimed in claim 1, wherein the temperature of vacuum drying in step (4) is 50-70 ℃, the drying time is 8-12 hours, and the vacuum degree is not more than 135 Pa.
5. The Te doped MXene potassium ion battery negative electrode material is characterized by being prepared by the preparation method of any one of claims 1-4.
6. The application of the Te doped MXene potassium ion battery negative electrode material in claim 5, wherein the Te doped MXene potassium ion battery negative electrode material is used for a potassium ion battery negative electrode.
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| CN109888279B (en) * | 2019-01-15 | 2022-01-04 | 五邑大学 | Selenium-doped MXene material and preparation method and application thereof |
| CN109830659B (en) * | 2019-01-15 | 2022-01-04 | 五邑大学 | Te-doped MXene material and preparation method thereof |
| CN109888203B (en) * | 2019-01-16 | 2022-01-04 | 五邑大学 | Tellurium-doped MXene composite material and preparation method and application thereof |
| CN112018354A (en) * | 2020-08-14 | 2020-12-01 | 五邑大学 | Array-shaped SnS2Preparation method of/MXene composite material |
| CN112072101A (en) * | 2020-08-14 | 2020-12-11 | 五邑大学 | Boron-doped MXene material and preparation method thereof |
| CN112018353A (en) * | 2020-08-14 | 2020-12-01 | 五邑大学 | WTE2/MXene composite material and preparation method thereof |
| CN113488638B (en) * | 2021-06-30 | 2022-12-23 | 肇庆市华师大光电产业研究院 | Preparation method of high-conductivity strong-adsorption lithium-sulfur battery positive electrode material |
| CN113437316B (en) * | 2021-07-06 | 2022-04-01 | 广东省武理工氢能产业技术研究院 | Tellurium-doped oxygen reduction catalyst and preparation method thereof |
| CN113745480B (en) * | 2021-08-28 | 2023-04-21 | 河南海宏科技有限公司 | Preparation method and application of layered two-dimensional material coated nickel-cobalt-manganese ternary positive electrode material |
| CN114477181A (en) * | 2022-01-26 | 2022-05-13 | 四川金时新能科技有限公司 | Method for rapidly preparing MXenes on large scale |
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