CN114195151A - Preparation method of single-layer MXene material - Google Patents
Preparation method of single-layer MXene material Download PDFInfo
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- 238000007710 freezing Methods 0.000 claims description 11
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- 238000001914 filtration Methods 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 4
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- 238000005119 centrifugation Methods 0.000 claims description 3
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- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
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- 238000005411 Van der Waals force Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
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- C01B21/00—Nitrogen; Compounds thereof
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Abstract
The invention relates to the technical field of two-dimensional layered materials, and particularly discloses a preparation method of a single-layer MXene material. The preparation method specifically comprises the following steps: mixing the multilayer MXene with a reducing solvent, reacting for 6-24 h at 90-180 ℃, washing, performing ultrasonic treatment, centrifuging, and drying to obtain the single-layer MXene material. The method is simple and feasible, a large amount of single-layer Mxene nanometer materials with uniform size and good dispersibility can be easily prepared, and the adopted reductive solvent is non-toxic and harmless, so that the physical structure and the electrical structure of the single-layer Mxene material can not be damaged.
Description
Technical Field
The invention relates to the technical field of two-dimensional layered materials, in particular to a preparation method of a single-layer MXene material.
Background
With the successful separation of monoatomic layer graphite materials, two-dimensional materials represented by graphene are rapidly developed and widely researched. Electrons in two-dimensional materials can move freely in only two dimensions, and have unique physical and chemical properties. In recent years, with the continuous research and exploration of two-dimensional materials, a family of two-dimensional materials is gradually enriched, including MXene, black phosphorus, transition metal sulfides, and the like, in addition to graphene.
MXene materials were commonly found by the professor Yury Gogotsi and the professor Michel Barsum in the United states in 2011, generally consist of layered transition metal carbides, nitrides or carbonitrides, and have the advantages of high specific surface area, high electrical conductivity, good optical and mechanical properties and the like. General formula M for MXene materialsn+1XnTxWherein M is a transition metal such as Ti, Sc, Mo, V or Cr; x is carbon, nitrogen or carbon nitrogen; t is a surface group such as-O, -OH, -F, etc.; the value of n is usually 1, 2, 3, etc., and the value of n is in positive correlation with the stability of the material. MAX phase is a precursor for preparing MXene, where A is a third or fourth main group element, and up to now more than 100 members of the MAX phase family have been reached, with conventional MAX phase materials including Ti3AlC2、Ti2AlC、V2AlC and Cr2AlC, and the like. The MAX phase has a hexagonal layered structure and consists of MX layers and A atomic layers which are alternately arranged, wherein the MX layers are bonded by metal bonds and van der Waals force exists between the MX layers and the A atomic layers, so that the M-A bonds have stronger chemical activity than the M-X bonds in the MAX phase, the bonding force of the M-A bonds is weaker, the A atoms can be selectively etched away, and finally, the MAX phase is obtained and corresponds to the MX layers and has a general formula of Mn+1XnThe multilayer laminate of (2). Due to van der waals force between two-dimensional MXene layers, self-stacking is easy to generate, the material performance is influenced, molecules are mostly inserted into the layers so as to enlarge the interlayer distance, but from the current research situation, the molecular intercalation and stripping efficiency is unsatisfactory, the main reason is due to insufficient power of molecular intercalation, and only a small part of intercalation reagent enters the layers of MXene. Therefore, a method for improving intercalation ability of intercalation agent is needed to solve the problem of insufficient power of molecular intercalation.
Disclosure of Invention
In view of this, the present application provides a method for preparing a single-layer MXene material, which uses a solvothermal intercalation method to achieve effective intercalation of a solvent and effective exfoliation of multiple layers of MXene molecules.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of a single-layer MXene material comprises the steps of mixing multiple layers of MXene with a reducing solvent, reacting for 6-24 hours at 90-180 ℃, washing, performing ultrasonic treatment, centrifuging, and drying to obtain the single-layer MXene material, wherein the reducing solvent is acetone, hydrazine hydrate, chloroform, isopropylamine, acetonitrile or ascorbic acid.
Compared with the prior art, the preparation method of the single-layer MXene material provided by the invention has the following advantages:
the method is simple and feasible, a large amount of single-layer Mxene nanometer materials with uniform size and good dispersibility can be easily prepared, and the adopted reductive solvent is non-toxic and harmless, so that the physical structure and the electrical structure of the single-layer Mxene material can not be damaged.
Due to the insufficient power of the current molecular intercalation, the applicant finds that the effective intercalation of the solvent and the effective stripping of the multi-layer MXene molecules can be realized under the temperature condition of 90-180 ℃ in the process of the solvent thermal intercalation through a large amount of researches, and the reasons for the effective intercalation and the effective stripping of the multi-layer MXene molecules may be as follows: the Gibbs free energy (Delta G) represents the driving force of solvent thermal intercalation, the entropy Delta S of intercalation reaction can be increased under a certain temperature condition, and for a mixed system of MXene and an organic solvent, the enthalpy Delta H of the intercalation reaction is generally a positive value due to Van der Waals attraction between two adjacent sheets in the MXene, so that under a certain high temperature condition, according to the Gibbs free energy (Delta G), the Delta G is equal to Delta H-T Delta S, the increasing Delta S can cause the value of Delta G to be reduced, and the value of Delta G is reduced, which indicates that the driving force of thermal intercalation is increased. Therefore, under a certain high temperature condition, the organic solvent can effectively overcome the van der Waals attraction between the MXene layers, and the solvent thermal intercalation of the multilayer MXene is realized to obtain the single-layer MXene material.
Optionally, the molecular formula of the multilayer MXene is Mn+1XnTxWherein M is an element Ti, Nb, V, Sc, Zr, Hf, Cr, Mo or Ta, X is an element C or N, N is 1, 2 or 3, and T is at least one of the surface groups-O, -OH or-F.
Optionally, the multiple layers of MXene are Ti3C2、Ti2C、Nb2C、V2C、V4C3、Ta4C3。
Optionally, the mass ratio of the reducing solvent to the multiple layers of MXene is 60-100: 1.
By selecting a specific reducing solvent and controlling the mass ratio of the solvent to the MXene, solvent molecules can slowly enter gaps of multiple MXene layers, the interlayer spacing of the multiple MXene layers is greatly improved, and interlayer solvent molecules or ions are removed by heating, so that the single-layer MXene material is obtained.
Optionally, the specific washing process includes sequentially washing with ethanol for 2 to 4 times, and washing with deionized water for 2 to 4 times.
The preferable washing condition can wash the solvent in the solvent hot-plug layer reaction liquid to provide a foundation for obtaining the single-layer MXene material with high purity at the later stage.
Optionally, the centrifugation conditions are: the rotating speed is 3000 rpm-4000 rpm, and the time is 50 min-70 min.
Further optionally, the conditions of the centrifugation are: the rotation speed is 3500rpm, and the time is 60 min.
Optionally, the ultrasonic conditions are as follows: the temperature is 0-5 ℃ for ice bath, the frequency is 35-45 kHz, and the time is 25-35 min.
Further optionally, the ultrasound conditions are: the temperature was 0 ℃ in an ice bath at a frequency of 40 kHz.
The preferred ultrasonic conditions are sufficient to disperse a monolayer of MXene material in water and form a colloidal solution with water.
Optionally, the drying is vacuum freeze drying, and the freezing temperature is-35 ℃ to-45 ℃.
Optionally, the preparation method of the multilayer MXene comprises the following steps: adding MAX phase raw materials into HF solution at the speed of 300-400 mg/min, stirring for 22-26 h at the temperature of 30-40 ℃, centrifuging, washing until the pH of supernatant is 6-8, and filtering to obtain multilayer MXene; the molecular formula of the MAX phase raw material is Mn+1AXnWherein M is an element Ti, Nb, V, Sc, Zr, Hf, Cr, Mo or Ta, wherein X is an element C or N, N is 1, 2 or 3, and A is Al, Si, Sn or Ge.
Optionally, the mass-to-volume ratio of the MAX phase raw material to the HF solution is (0.5-1.5): 10, the unit of the mass is g, and the unit of the volume is ml; the mass concentration of the HF solution is 45-55%.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows a single Ti layer prepared in example 1 of the present invention3C2TxAn XRD pattern of the material;
FIG. 2 shows a single Ti layer prepared in example 1 of the present invention3C2TxTEM photograph of the material;
FIG. 3 is a TEM photograph of a material prepared in comparative example 1 of the present invention;
FIG. 4 is a TEM photograph of a material prepared in comparative example 2 of the present invention;
FIG. 5 is a TEM photograph of a material prepared in comparative example 3 of the present invention;
FIG. 6 shows a single Ti layer prepared in example 1 of the present invention3C2TxAn optical photograph of the material;
FIG. 7 shows an AFM spectrum provided in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Ti3AlC2Adding the phase raw material into 20ml of 49% HF solution at the speed of 400mg/min, stirring for 24h at the temperature of 35 ℃, centrifuging, washing by using deionized water until the pH of the supernatant is 7, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer Ti3C2Tx;
Step two, a plurality of layers of Ti3C2TxPlacing the mixture in a polytetrafluoroethylene hydrothermal reaction kettle, adding acetone, reacting for 18h at 120 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasound at 0 ℃ for 30min, wherein the ultrasound frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain the monolayer Ti3C2TxMaterial of, among others, acetone with multiple layers of Ti3C2TxIn a mass ratio of 60: 1.
Example 2
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Ti2Adding AlC phase raw material into 20ml HF solution with mass concentration of 49% at the speed of 300mg/min, stirring for 22h at the temperature of 40 ℃, centrifuging, washing with deionized water until the pH of supernatant is 6, and vacuum-filtering with organic filter membrane to obtain multilayer Ti2CTx;
Step two, a plurality of layers of Ti2CTxPutting the mixture into a polytetrafluoroethylene hydrothermal reaction kettle, adding hydrazine hydrate, reacting for 12 hours at 120 ℃, washing for 4 times by using ethanol, washing for 2 times by using deionized water, carrying out ice bath ultrasonic treatment at 0 ℃ for 35min, wherein the ultrasonic frequency is 35kHz, centrifuging for 70min at the rotating speed of 3000rpm, carrying out vacuum freeze drying at the freezing temperature of-35 ℃ to obtain the single-layer Ti2CTxMaterial of, among others, hydrazine hydrate with multiple layers of Ti2CTxIn a mass ratio of 60: 1.
Example 3
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Nb2Adding AlC phase raw material into 13ml of 49% HF solution at the speed of 350mg/min, stirring for 26h at the temperature of 30 ℃, centrifuging, washing by using deionized water until the pH of supernatant is 8, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer Nb2CTx;
Step two, multiple Nb layers2CTxPlacing the mixture into a polytetrafluoroethylene hydrothermal reaction kettle, adding chloroform, reacting for 24h at 90 ℃, washing for 2 times by using ethanol, washing for 4 times by using deionized water, carrying out ice bath ultrasound at 0 ℃ for 25min, wherein the ultrasound frequency is 45kHz, centrifuging for 50min at the rotating speed of 4000rpm, carrying out vacuum freeze drying at the freezing temperature of-45 ℃ to obtain the single-layer Nb2CTxMaterial of chloroform with multiple layers of Nb2CTxIn a mass ratio of 60: 1.
Example 4
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g V2Adding AlC phase raw material into 20ml HF solution with mass concentration of 49% at a speed of 350mg/min, stirring for 24h at a temperature of 35 ℃, centrifuging, washing with deionized water until the pH of supernatant is 7, and vacuum-filtering with organic filter membrane to obtain multilayer V2CTx;
Step two, a plurality of layers V2CTxPlacing the mixture into a polytetrafluoroethylene hydrothermal reaction kettle, adding isopropylamine, reacting for 9h at 150 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasonic treatment at 3 ℃ for 30min, wherein the ultrasonic frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain the monolayer V2CTxMaterial of, inter alia, isopropylamine with multilayers V2CTxThe mass ratio of (A) to (B) is 80: 1.
Example 5
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g V4AlC3Adding the phase raw material into 30ml of 49% HF solution at the speed of 300mg/min, stirring for 24h at the temperature of 36 ℃, centrifuging, washing by using deionized water until the pH of the supernatant is 6, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer V4C3Tx;
Step two, a plurality of layers V4C3TxPlacing the mixture in a polytetrafluoroethylene hydrothermal reaction kettle, adding acetonitrile, reacting for 6h at 180 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasound at 5 ℃ for 30min, wherein the ultrasound frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain the monolayer V4C3TxMaterial of, among others, acetonitrile with multilayers V4C3TxThe mass ratio of (A) to (B) is 100: 1.
Example 6
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Ta4AlC3Adding the phase raw material into 25ml of 49% HF solution at the speed of 400mg/min, stirring for 24h at the temperature of 34 ℃, centrifuging, washing by using deionized water until the pH of the supernatant is 7, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer Ta4C3Tx;
Step two, providing a plurality of layers of Ta4C3TxPlacing the mixture into a polytetrafluoroethylene hydrothermal reaction kettle, adding ascorbic acid, reacting for 13h at 110 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasonic treatment at 0 ℃ for 30min, wherein the ultrasonic frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain the single-layer Ta4C3TxMaterial of, wherein ascorbic acid is present with a plurality of layers of Ta4C3TxQuality of (1)The quantity ratio is 70: 1.
Example 7
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Ti2Adding AlN phase raw material into 20ml of HF solution with the mass concentration of 49% at the speed of 400mg/min, stirring for 24 hours at the temperature of 35 ℃, centrifuging, washing by using deionized water until the pH of supernatant is 7, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer Ti2NTx;
Step two, a plurality of layers of Ti2NTxPlacing the mixture in a polytetrafluoroethylene hydrothermal reaction kettle, adding acetone, reacting for 18h at 120 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasound at 0 ℃ for 30min, wherein the ultrasound frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain the monolayer Ti2NTxMaterial of, among others, acetone with multiple layers of Ti2NTxIn a mass ratio of 60: 1.
Example 8
The embodiment provides a preparation method of a single-layer MXene material, which comprises the following steps:
step one, 2g of Ti4AlN3Adding the phase raw material into 20ml of 49% HF solution at the speed of 300mg/min, stirring for 22h at the temperature of 40 ℃, centrifuging, washing by using deionized water until the pH of the supernatant is 6, and performing vacuum filtration by using an organic filter membrane to obtain a multilayer Ti4N3Tx;
Step two, a plurality of layers of Ti4N3TxPutting the mixture into a polytetrafluoroethylene hydrothermal reaction kettle, adding hydrazine hydrate, reacting for 12 hours at 120 ℃, washing for 4 times by using ethanol, washing for 2 times by using deionized water, carrying out ice bath ultrasonic treatment at 0 ℃ for 35min, wherein the ultrasonic frequency is 35kHz, centrifuging for 70min at the rotating speed of 3000rpm, carrying out vacuum freeze drying at the freezing temperature of-35 ℃ to obtain the single-layer Ti4N3TxMaterial of, among others, hydrazine hydrate with multiple layers of Ti4N3TxIn a mass ratio of 60: 1.
In order to better illustrate the technical solution of the present invention, further comparison is made below by means of a comparative example and an example of the present invention.
Comparative example 1
The multilayer Ti obtained in example 13C2Tx(ii) a Carrying out hot solvent intercalation, replacing the reaction temperature with 220 ℃, and keeping the rest conditions unchanged, wherein the specific process comprises the following steps:
a plurality of layers of Ti3C2TxPlacing in a polytetrafluoroethylene hydrothermal reaction kettle, adding acetone, reacting for 18h at 220 ℃, washing for 3 times by using ethanol, washing for 3 times by using deionized water, carrying out ice bath ultrasound at 0 ℃ for 30min, wherein the ultrasound frequency is 40kHz, centrifuging for 60min at the rotating speed of 3500rpm, carrying out vacuum freeze drying at the freezing temperature of-40 ℃ to obtain a product, wherein the acetone and the Ti are mixed to obtain the final product3C2In a mass ratio of 60: 1.
Comparative example 2
The multilayer Ti obtained in example 13C2Tx(ii) a Carrying out hot solvent intercalation, replacing the reaction temperature with 70 ℃, and keeping the rest conditions unchanged, wherein the specific process comprises the following steps:
a plurality of layers of Ti3C2TxPlacing in a polytetrafluoroethylene hydrothermal reaction kettle, adding acetone, reacting at 70 ℃ for 18h, washing with ethanol for 3 times, washing with deionized water for 3 times, carrying out ice bath ultrasound at 0 ℃ for 30min, wherein the ultrasound frequency is 40kHz, centrifuging at 3500rpm for 60min, and carrying out vacuum freeze drying at-40 ℃ to obtain a product, wherein the acetone and Ti are mixed to obtain the final product3C2In a mass ratio of 60: 1.
Comparative example 3
The multilayer Ti obtained in example 13C2Tx(ii) a Carrying out thermal solvent intercalation, replacing the solvent with tetrabutyl ammonium hydroxide, and keeping the other conditions unchanged, wherein the specific process comprises the following steps:
a plurality of layers of Ti3C2TxPlacing in a polytetrafluoroethylene hydrothermal reaction kettle, adding tetrabutylammonium hydroxide, reacting at 120 deg.C for 18h, washing with ethanol for 3 times, washing with deionized water for 3 times, performing ultrasonic treatment at 0 deg.C in ice bath for 30min,ultrasonic frequency of 40kHz, centrifuging at 3500rpm for 60min, vacuum freeze drying at-40 deg.C to obtain product containing tetrabutylammonium hydroxide and Ti layers3C2TxIn a mass ratio of 60: 1.
To better illustrate the monolayer M provided by the embodiments of the present inventionn+1XnTxThe following tests were conducted on the properties of the materials prepared in example 1 and comparative examples 1 to 3.
Experimental example 1 XRD
For the single layer Ti prepared in example 13C2TxXRD was performed for analysis, and the results are shown in FIG. 1.
As can be seen from fig. 1, diffraction peaks appear at 8.90 °, 18.26 °, 25.28 °, 27.48 °, 35.97 °, 41.78 ° and 60.72 ° of 2 θ, which correspond to the (002), (004), (005), (007), (008), (0012) and (110) crystal planes, respectively, and thus it can be seen that the product prepared in example 1 of the present application is Ti3C2TxA material.
Experimental example 2 TEM
TEM analysis of the materials prepared in example 1 and comparative examples 1 to 3 is shown in FIGS. 2 to 5.
As can be seen from FIG. 2, the product produced in example 1 of the present invention is indeed a monolayer of Ti3C2TxA material.
As can be seen from FIGS. 3 to 5, the materials prepared in comparative examples 1 to 3 are all multilayer, so that a specific temperature range and a specific reducing agent are selected to realize effective intercalation of the solvent and effective stripping of multiple MXene molecules.
Test example 3 optical detection
The centrifugate obtained in the second step of example 1 was optically detected, and the results are shown in FIG. 6. As can be seen from FIG. 6, the centrifugate prepared in example 1 contains a monolayer of Ti3C2TxThe Tyndall effect was observed for dispersions of the material, indicating a monolayer of Ti3C2TxThe material forms a colloidal solution with water, demonstrating a monolayer of Ti3C2TxThe material has good dispersibility in water.
Test example 4 AFM detection
The single layer Ti prepared in example 13C2TxAFM analysis was performed, and the results are shown in FIG. 7.
As can be seen from FIG. 7, the single layer Ti prepared in the present application3C2TxIs 4.55 nm.
Examples 2 to 8 prepared Mn+1XnTxThe thickness of the material was substantially the same as in example 1, i.e. the materials prepared were all single layers Mn+1XnTxA material.
Examples 2 to 8 prepared Mn+1XnTxThe material can form a colloidal solution in water, and the same or corresponding technical effect as that of the embodiment 1 can be achieved.
As long as the M element, the X element and the A element in the MAX phase raw material are within the preferable range of the invention, the same or corresponding technical effects of the embodiments 1-8 of the invention can be achieved, and the prepared products are all single-layer Mn+1XnTxA material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a single-layer MXene material is characterized by comprising the following steps: mixing the multilayer MXene with a reducing solvent, reacting for 6-24 h at 90-180 ℃, washing, performing ultrasonic treatment, centrifuging, and drying to obtain the single-layer MXene material, wherein the reducing solvent is acetone, hydrazine hydrate, chloroform, isopropylamine, acetonitrile or ascorbic acid.
2. The method for preparing the single-layer MXene material of claim 1, wherein: the molecular formula of the multilayer MXene is Mn+1XnTxWherein M is elements Ti and NbV, Sc, Zr, Hf, Cr, Mo or Ta, X is an element C or N, N is 1, 2 or 3, and T is at least one of the surface groups-O, -OH or-F.
3. The method for preparing a single layer MXene material of claim 2, wherein: the multilayer MXene is Ti3C2、Ti2C、Nb2C、V2C、V4C3、Ta4C3。
4. The method for preparing the single-layer MXene material of claim 1, wherein: the mass ratio of the reducing solvent to the multiple layers of MXene is 60-100: 1.
5. The method for preparing the single-layer MXene material of claim 1, wherein: the specific washing process comprises the steps of sequentially washing for 2-4 times by adopting ethanol and washing for 2-4 times by adopting deionized water.
6. The method for preparing the single-layer MXene material of claim 1, wherein: the centrifugation conditions were: the rotating speed is 3000 rpm-4000 rpm, and the time is 50 min-70 min.
7. The method for preparing the single-layer MXene material of claim 1, wherein: the ultrasonic conditions are as follows: the temperature is 0-5 ℃ for ice bath, the frequency is 35-45 kHz, and the time is 25-35 min.
8. The method for preparing the single-layer MXene material of claim 1, wherein: the drying adopts vacuum freeze drying, and the freezing temperature is-35 ℃ to-45 ℃.
9. The method for preparing the single-layer MXene material according to any one of claims 1 to 8, wherein: the preparation method of the multilayer MXene comprises the following steps: adding MAX phase raw material into HF solution at the speed of 300-400 mg/min, stirring at 30-40 deg.C for 22-26 h,centrifuging, washing until the pH value of the supernatant is 6-8, and filtering to obtain a multilayer MXene; the molecular formula of the MAX phase raw material is Mn+1AXnWherein M is an element Ti, Nb, V, Sc, Zr, Hf, Cr, Mo or Ta, wherein X is an element C or N, N is 1, 2 or 3, and A is Al, Si, Sn or Ge.
10. The method for preparing a single layer MXene material of claim 9, wherein: the mass-volume ratio of the MAX phase raw material to the HF solution is (0.5-1.5): 10, the unit of the mass is g, and the unit of the volume is ml; and/or
The mass concentration of the HF solution is 45-55%.
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