CN115676831A - Porous MXene material and preparation method and application thereof - Google Patents
Porous MXene material and preparation method and application thereof Download PDFInfo
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- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 17
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a porous MXene material and a preparation method and application thereof, and belongs to the technical field of MXene materials. The invention provides a preparation method of a porous MXene material, which comprises the following steps: and carrying out spray pyrolysis on the MXene dispersion liquid to obtain the porous MXene material. Aiming at the problems that MXene has a multilayer stacked structure and small interlayer spacing and is used as a negative electrode material of a lithium ion battery in the prior art, the rapid reversible embedding/removing of metal ions is seriously hindered, the MXene dispersion liquid is atomized by an atomizer and is carried into a high-temperature tube furnace by carrier gas for heating in a spray cracking mode to prepare the porous wrinkled MXene material, the conductivity is better, the interlayer spacing is large, the specific surface area is increased, the lithium ion transmission is more convenient, and the porous MXene material with high ion, electronic conductivity and excellent electrochemical performance is obtained.
Description
Technical Field
The invention relates to the technical field of MXene materials, in particular to a porous MXene material and a preparation method and application thereof.
Background
Layered materials have unusual physical properties and excellent electrical properties. Most importantly, the ultra-high surface area exposed makes it very versatile. Among layered materials, carbon materials having a two-dimensional or quasi-two-dimensional morphology are widely used in the fields of catalysis, water/gas purification, energy conversion/storage, and the like, due to the inherent advantages of large specific surface area, excellent conductivity, chemical inertness, low cost, and the like.
However, two-dimensional structure carbon materials face the problem of severe agglomeration, which limits ion accessibility, diffusion and mass transport, especially after being prepared into electrodes in the field of electrochemical energy storage. In order to solve the above problems, many researchers have been working on reconstructing a two-dimensional carbon material by designing a structure such as a three-dimensional porous membrane, a scaffold and a network to increase an ion-contactable surface area and improve ion transport efficiency. Common methods include preparing pleated nanoplates or incorporating nanoparticles of small size into the nanoplates such that interlayer spaces can be created when these nanoparticles are packed together.
MXene is a two-dimensional inorganic compound composed of a transition metal carbide, nitride or carbonitride, which has a multilayer structure and excellent electronic conductivity. However, MXene generally exhibits a thermodynamically metastable state with a high surface energy due to the high proportion of exposed metal atoms on the surface. At a certain temperature, even if protective gas (nitrogen and argon) is introduced in the preparation process, trace oxygen in the protective gas can still react with oxygen-containing groups existing on the surface of MXene to be spontaneously converted into more stable metal oxide, and the surface oxidation can cause the reduction of the conductivity and the passivation of a reaction interface. The common methods for preparing the micro-nano materials, such as water/solvent thermal synthesis, reflux, calcination and the like, are difficult to avoid.
Disclosure of Invention
In view of this, the invention aims to provide a porous MXene material, and a preparation method and application thereof. The porous MXene material prepared by the method has high conductivity and excellent electrochemical performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a porous MXene material, which comprises the following steps:
and carrying out spray pyrolysis on the MXene dispersion liquid to obtain the porous MXene material.
Preferably, the temperature of the spray cracking is 400-1000 ℃, the carrier gas is nitrogen, and the flow rate of the carrier gas is 200-400 sccm.
Preferably, the MXene dispersion liquid further comprises an interlayer spacing agent, wherein the interlayer spacing agent comprises one or more of metal oxide, metal nitride, glucose and graphene oxide.
Preferably, the mass ratio of the MXene nanosheets to the interlayer spacing agent in the MXene dispersion liquid is (0.5-2.5): 1.
preferably, the mass ratio of the MXene nanosheets to the interlayer spacing agent in the MXene dispersion liquid is (1-2): 1.
preferably, when the interlayer spacing agent is glucose and/or graphene oxide, the temperature of the spray pyrolysis is 400-600 ℃, the carrier gas is nitrogen, and the flow rate of the carrier gas is 200-400 sccm.
Preferably, MXene in the MXene dispersion comprises Ti 3 C 2 T x 、Ti 2 CT x 、V 2 CT x 、Mo 2 CT x 、Nb 2 CT x 、Nb 4 C 3 T x 、Cr 2 CT x 、Mo 2 TiC 2 T x And Mo 2 Ti 2 C 3 T x Wherein T is x Including one or more of-F, -Cl, -OH and-O.
Preferably, MXe is in the MXene dispersionThe mass concentration of ene is 2-5 mg/mL -1 。
The invention also provides the porous MXene material prepared by the preparation method in the technical scheme.
The invention also provides application of the porous MXene material in the technical scheme as a lithium ion battery cathode material.
The invention provides a preparation method of a porous MXene material, which comprises the following steps: and carrying out spray pyrolysis on the MXene dispersion liquid to obtain the porous MXene material.
Aiming at the problems that MXene has a multilayer stacked structure and small interlayer spacing and is used as a negative electrode material of a lithium ion battery in the prior art, the rapid reversible embedding/removing of metal ions is seriously hindered, the MXene dispersion liquid is atomized by an atomizer and is carried into a high-temperature tube furnace by carrier gas for heating in a spray cracking mode to prepare the porous wrinkled MXene material, the conductivity is better, the interlayer spacing is large, the specific surface area is increased, the lithium ion transmission is more convenient, and the porous MXene material with high ion, electronic conductivity and excellent electrochemical performance is obtained.
Furthermore, the MXene dispersion liquid also comprises an interlayer spacing agent, so that the interlayer spacing is further increased, the conductivity is better, the specific surface area is larger, and the lithium ion transmission is more convenient.
The invention also provides the porous MXene material prepared by the preparation method in the technical scheme.
Drawings
In FIG. 1, a is an SEM image of a porous MXene-SP material, and b is 0.1 A.g of MXene-SP serving as a lithium ion battery negative electrode material -1 A plot of cycling performance at current density;
in FIG. 2, a is SEM picture of porous MXene/C-SP material, and b is 0.1 A.g of MXene/C-SP as negative electrode material of lithium ion battery -1 A plot of cycling performance at current density;
FIG. 3 is an SEM image of a porous MXene/rGO-SP material at different magnifications;
in fig. 4, a is an SEM image of the MXene powder material in example 4, and b is the MXene powder material in example 4 as the negative electrode material of the lithium ion batteryAt 0.1 A.g -1 Cycling performance plot at current density.
Detailed Description
The invention provides a preparation method of a porous MXene material, which comprises the following steps:
and carrying out spray pyrolysis on the MXene dispersion liquid to obtain the porous MXene material.
In the present invention, unless otherwise specified, all the raw materials used are commercially available in the art.
In the present invention, the temperature of the spray pyrolysis is preferably 400 to 1000 ℃, the carrier gas is preferably nitrogen, and the flow rate of the carrier gas is preferably 200 to 400sccm.
In the present invention, the MXene dispersion preferably further includes an interlayer spacer, and the interlayer spacer preferably includes one or more of a metal oxide, a metal nitride, glucose, and graphene oxide.
In the present invention, the ratio by mass of the MXene nanoplatelets to the interlaminar spacing agent in the MXene dispersion is preferably (0.5 to 2.5): 1, more preferably (1 to 2): 1.
in the present invention, when the interlayer spacer is preferably glucose and/or graphene oxide, the temperature of the spray pyrolysis is preferably 400 to 600 ℃, the carrier gas is preferably nitrogen, and the flow rate of the carrier gas is preferably 200 to 400sccm.
When the interlayer spacing agent preferably comprises one or more of a metal oxide, a metal nitride and glucose, the interlayer spacing agent is preferably directly mixed with the MXene dispersion.
When the interlayer spacer preferably includes graphene oxide, the graphene oxide is preferably added in the form of an aqueous graphene oxide solution.
When the MXene dispersion liquid preferably comprises an interlayer spacing agent, ultrasonic treatment is preferably carried out before spray cracking, the power of the ultrasonic treatment is preferably 100W, and the time is preferably 0.5-2 h.
In the present invention, MXene in the MXene dispersion preferably includes Ti 3 C 2 T x 、Ti 2 CT x 、V 2 CT x 、Mo 2 CT x 、Nb 2 CT x 、Nb 4 C 3 T x 、Cr 2 CT x 、Mo 2 TiC 2 T x And Mo 2 Ti 2 C 3 T x Wherein T is x Including one or more of-F, -Cl, -OH and-O.
In the present invention, the MXene dispersion is preferably prepared by using Ti in the present invention 3 C 2 T x The preparation of MXene dispersions is described by way of example and preferably comprises the following steps:
weighing Ti 3 AlC 2 Putting the precursor into a polytetrafluoroethylene beaker, adding an HF solution, stirring and reacting for 18-24 h, centrifuging and washing for 5-6 times by using distilled water, adding a tetrabutylammonium hydroxide solution, stirring for 24h at room temperature, centrifuging and washing for 3 times by using distilled water, adding 200mL of distilled water, introducing nitrogen, performing ultrasonic treatment for 4-6 h at 100W power, centrifuging at the rotating speed of 3500-5000 rpm for 2-10 min, and collecting an upper-layer dispersion liquid to obtain the MXene dispersion liquid.
In a specific embodiment of the present invention, the method for preparing the MXene dispersion comprises the following steps:
weighing 2gTi 3 AlC 2 Placing the precursor in a polytetrafluoroethylene beaker, slowly adding 20mL of 35wt% HF solution, stirring and reacting for 18-24 h, centrifuging and washing for 5-6 times by using distilled water, adding 25mL of 40wt% tetrabutylammonium hydroxide solution, stirring for 24h at room temperature, centrifuging and washing for 3 times by using distilled water, adding 200mL of distilled water, introducing nitrogen, performing ultrasonic treatment for 4-6 h at 100W power, centrifuging at the rotating speed of 3500-5000 rpm for 2-10 min, and collecting upper-layer dispersion liquid to obtain the MXene dispersion liquid.
In the present invention, the concentration by mass of MXene in the MXene dispersion is preferably 2 to 5 mg/mL -1 More preferably 2 to 4 mg/mL -1 。
The invention also provides the porous MXene material prepared by the preparation method in the technical scheme.
The invention also provides application of the porous MXene material in the technical scheme as a lithium ion battery cathode material.
The invention is not particularly limited to the specific manner of use described, as such may be readily adapted by those skilled in the art.
In order to further illustrate the present invention, the following detailed description of the porous MXene material and the preparation method and application thereof are provided in connection with examples, which should not be construed as limiting the scope of the present invention.
Example 1
Preparation of porous Mxene-SP material and electrochemical performance thereof
Weighing 2gTi 3 AlC 2 Placing the precursor in a polytetrafluoroethylene beaker, slowly adding 20mL of 35wt% HF solution, stirring and reacting for 24h, centrifuging and washing for 6 times by using distilled water, adding 25mL of 40wt% tetrabutylammonium hydroxide solution, stirring for 24h at room temperature, centrifuging and washing for 3 times by using distilled water, adding 200mL of distilled water, introducing nitrogen, performing ultrasonic treatment for 6h at 100W power, centrifuging at the rotating speed of 5000rpm for 10min, and collecting an upper-layer dispersion liquid to obtain the MXene dispersion liquid.
50mL of MXene dispersion liquid is taken, 50mL of distilled water is added for dilution, and then the porous MXene-SP material is prepared through spray pyrolysis, wherein the pyrolysis temperature is 400 ℃, the carrier gas is nitrogen, and the carrier gas flow rate is 200sccm.
The prepared porous MXene-SP material is subjected to SEM test. As shown in a in FIG. 1, it can be seen that the porous MXene-SP has a highly wrinkled and porous morphology.
Uniformly grinding the prepared MXene-SP material, acetylene black and polyvinylidene fluoride (PVDF) according to the mass ratio of 8. The method comprises the steps of taking metal lithium as a counter electrode and a reference electrode, taking an electrode material as a working electrode, taking a polypropylene membrane as a diaphragm, and taking 1M LiPF 6 Is an electrolyte, and is assembled into a button cell in a glove box with the water oxygen concentration of less than 0.01 ppm. The electrochemical performance test adopts a blue battery test system, and MXene-SP is used as a lithium ion battery cathode material at 0.1 A.g -1 Cycling at Current DensityThe ring performance is shown in b in FIG. 1, and it is found that MXene-SP material is at 0.1A · g -1 The reversible specific capacity under the current density is 1104 mAh.g -1 And 733.1mAh g still remain after 100 cycles of circulation -1 And the electrochemical performance and the cycling stability are excellent.
Example 2
MXene dispersion was prepared in the same manner as in example 1.
Taking 50mL of MXene dispersion, adding 50mL of distilled water for dilution, then adding 100mg of glucose, carrying out 100W ultrasound for 2h, and preparing a porous MXene/C-SP material by spray cracking at the cracking temperature of 600 ℃, wherein the carrier gas is nitrogen and the flow rate of the carrier gas is 400sccm.
In FIG. 2, a is SEM picture of porous MXene/C-SP material, and b is 0.1 A.g of MXene/C-SP as negative electrode material of lithium ion battery -1 The cycle performance diagram under the current density shows that the MXene/C-SP material presents a highly-wrinkled and porous appearance, the lamellar structure contains small particles, and the lithium ion battery taking the MXene/C-SP as the negative electrode material has the concentration of 0.1 A.g -1 The lower reversible specific capacity is 780.3 mAh.g -1 And the 506.2mAh g still remains after 100 cycles of circulation -1 And exhibits excellent cycle stability.
Example 3
The MXene dispersion was prepared in the same manner as in example 1.
Taking 50mL of MXene dispersion liquid, adding 50mL of distilled water for dilution, then adding 10mL of graphene oxide solution with the concentration of 1mg/mL, carrying out ultrasonic treatment for 2 hours at 100W, and carrying out spray pyrolysis to prepare a porous MXene/rGO-SP material, wherein the pyrolysis temperature is 600 ℃, the carrier gas is nitrogen, and the carrier gas flow rate is 200sccm.
FIG. 3 is SEM images of porous MXene/rGO-SP materials at different magnifications, and it can be seen from the SEM images that the MXene/rGO-SP materials present a highly wrinkled and porous appearance, and fine particles are contained on a lamellar structure.
The content of lithium ion battery taking MXene/rGO-SP as negative electrode material is 0.1 A.g -1 The lower reversible specific capacity is 739.6 mAh.g -1 And 488.7mAh g is still remained after 100 cycles of circulation -1 And exhibits excellent cycle stability.
Example 4
MXene dispersion was prepared in the same manner as in example 1.
And (3) freeze-drying the MXene dispersion liquid to obtain an MXene powder material.
In FIG. 4, a is the SEM picture of MXene powder material in example 4, and b is 0.1 A.g.of MXene powder material in example 4 as negative electrode material of lithium ion battery -1 The cycle performance graph under current density shows that MXene powder material presents the appearance of layered stacking in an SEM (scanning electron microscope) picture, and the content of the MXene powder material in a lithium ion battery taking the MXene powder material as a negative electrode material is 0.1 A.g -1 The lower reversible specific capacity is only 556.5mAh g -1 And after 100 cycles, the capacity is attenuated to 339.7mAh g -1 。
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. The preparation method of the porous MXene material is characterized by comprising the following steps:
and carrying out spray pyrolysis on the MXene dispersion liquid to obtain the porous MXene material.
2. The method according to claim 1, wherein the temperature of the spray pyrolysis is 400 to 1000 ℃, the carrier gas is nitrogen, and the flow rate of the carrier gas is 200 to 400sccm.
3. The preparation method of claim 1, wherein the MXene dispersion liquid further comprises an interlayer spacer, and the interlayer spacer comprises one or more of a metal oxide, a metal nitride, glucose and graphene oxide.
4. The preparation method according to claim 3, wherein the MXene dispersion liquid comprises MXene nanosheets and interlayer spacing agent in a mass ratio of (0.5-2.5): 1.
5. the preparation method according to claim 4, wherein the MXene dispersion liquid comprises MXene nanosheets and interlayer spacing agent in a mass ratio of (1-2): 1.
6. the preparation method according to claim 3, wherein when the interlayer spacing agent is glucose and/or graphene oxide, the temperature of the spray pyrolysis is 400 to 600 ℃, the carrier gas is nitrogen, and the flow rate of the carrier gas is 200 to 400sccm.
7. The method according to claim 1, wherein MXene in the MXene dispersion liquid comprises Ti 3 C 2 T x 、Ti 2 CT x 、V 2 CT x 、Mo 2 CT x 、Nb 2 CT x 、Nb 4 C 3 T x 、Cr 2 CT x 、Mo 2 TiC 2 T x And Mo 2 Ti 2 C 3 T x Wherein T is x Including one or more of-F, -Cl, -OH and-O.
8. The preparation method according to claim 1, wherein the mass concentration of MXene in the MXene dispersion liquid is 2-5 mg-mL -1 。
9. A porous MXene material obtained by the production method according to any one of claims 1 to 8.
10. Use of the porous MXene material of claim 9 as a negative electrode material for lithium ion batteries.
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| CN113834863A (en) * | 2021-09-24 | 2021-12-24 | 吉林大学 | Based on three-dimensional Ti3C2Room temperature high selectivity NO of Tx/rGO composite folded ball2Sensor and preparation method |
Cited By (4)
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