CN111302343A - MXene nanotube and general synthesis method thereof - Google Patents
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Abstract
An MXene nanotube and a general synthetic method thereof, belonging to the field of nano materials. The MXene nanotube is formed by axially overlapping two-dimensional MXene in a staggered manner, the outer diameter of the MXene nanotube is 0.5-1 μm, and the wall thickness of the MXene nanotube is 0.02-0.1 μm. The preparation method comprises the following steps: preparing MXene/polymer composite fiber with a core-shell structure by using an electrostatic spinning machine, and removing the sacrificial template at the temperature of 600-700 ℃ to obtain the MXene nanotube with controllable structure and size. The MXene nanotube obtained by the invention overcomes the basic problem that two-dimensional MXene is easy to stack and agglomerate under Van der Waals force, has the advantages of large specific surface area, simple and controllable preparation method, good economy and the like, and lays a foundation for preparation, processing and application in various aspects of MXene-based high-performance functional materials. Meanwhile, MXene nanotubes are crosslinked with each other to form a flexible three-dimensional assembly, so that the application of the MXene material in the fields of wearable flexible energy devices, electromagnetic shielding, wave-absorbing materials and the like is expanded.
Description
Technical Field
The invention belongs to the field of nano materials, and relates to an MXene nanotube and a general synthetic method thereof.
Background
The nano material has a unique size effect, has a larger active area, a shorter ion and electron transmission distance and excellent physicochemical properties compared with a bulk material, and is widely applied in various fields. The performance of the functional nano material depends on the appearance, size and crystalline phase structure of the functional nano material to a great extent, the microstructure of the functional nano material is finely regulated, and the realization of structural design and controllable construction become the hot field of scientific research of nano materials in recent years.
MXene is a novel two-dimensional crystal of transition metal carbide or nitride, and has a two-dimensional structure similar to graphene. Having the chemical formula Mn+1Xn(n is 1,2,3, M is a transition metal element, and X is carbon or nitrogen). The material is obtained by selectively etching the MAX phase of the layered ceramic material by acid, has excellent electrical, mechanical and magnetic properties, and has great application potential in the fields of energy storage, intelligent wearing, electromagnetic shielding and the like. The one-dimensional nanotube structure has the advantages of high porosity, high specific surface area and the like, and has wide application prospects in the fields of adsorption, catalysis, electrochemistry and the like. However, the one-dimensional MXene nanotube has not achieved any progress so far, which seriously affects and limits the macroscopic performance and the processing performance of MXene in various fields.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an MXene nanotube and a general synthesis method thereof, and the prepared MXene nanotube is formed by overlapping two-dimensional MXene sheets in an axially staggered manner along the nanotube. The MXene nanotube prepared by the method has the advantages of large specific surface area, high conductivity, good flexibility, economy, effectiveness and large-scale application, and fundamentally solves the fundamental problem which puzzles MXene performance exertion and various applications.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an MXene nanotube is prepared from two-dimensional MXene sheets through axially and alternatively lapping, and has external diameter of 0.5-1 μ M and wall thickness of 0.02-0.1 μ M, and general structural formula of MXene nanotuben+1XnOr (M)1,M2)n+1XnOr Mn+1(X1,X2)nOne or a combination of two or more of them.
Said Mn+1XnWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x ═ C, N.
Said (M)1,M2)n+1XnIn, M1,M2＝Ti,Nb,V,Mo,Zr,Cr,W,Ta；n＝1,2,3；X＝C,N。
Said Mn+1(X1,X2)nWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x1,X2＝C,N。
A general preparation method of MXene nanotubes specifically comprises the following steps:
1) dispersing MXene in N, N-dimethylformamide under normal temperature and pressure to obtain dispersion with concentration of 10-60mg mL-1。
2) Dissolving polyacrylonitrile in the MXene dispersion liquid prepared in the step 1) at the temperature of 50-60 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 100-120mg mL-1。
3) The sacrificial template agent is dissolved in N, N-dimethylformamide at the temperature of 60-75 ℃ to form a homogeneous solution. The concentration of the sacrificial template solution is 200-250mg mL-1. The sacrificial template is polymethyl methacrylateOne or a mixture of more of polystyrene and polyvinylpyrrolidone.
4) Filling the mixed solution obtained in the step 2) into an injector A, filling the solution obtained in the step 3) into an injector B, and performing coaxial electrostatic spinning by using an electrostatic spinning machine, wherein the mixed solution obtained in the step 2) is an outer-layer solution, and the propelling speed is 1.0-1.2mlh-1The solution in the step 3) is an inner layer solution, and the advancing speed is 0.8-1.0ml h-1The voltage of the positive electrode is 18-22kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 15-18cm, and a rotating metal roller is used as a collecting device.
5) Annealing the material collected in the step 4) by using a tubular furnace at the temperature of 600-700 ℃ for 1-2h to obtain the MXene nanotube.
Compared with the prior art, the invention solves the problems of preparation, processing and application of the two-dimensional MXene, and has the beneficial effects that:
(1) in the nanotube structure, two-dimensional MXene sheets are overlapped in an staggered mode along the axial direction, stacking and agglomeration caused by Van der Waals interaction between MXenes can be inhibited, and the interface of the MXene sheets is efficiently utilized.
(2) The method can realize fine regulation and control of the structure and the size of the MXene nanotube, and has the advantages of large specific surface area, simple and controllable preparation method and good economy.
(3) The MXene nanotubes are mutually crosslinked to form a flexible three-dimensional assembly, so that the application of the MXene material in the fields of wearable flexible energy devices, electromagnetic shielding, wave-absorbing materials and the like is expanded.
Drawings
FIG. 1 is a scanning electron micrograph of MXene nanotubes prepared in example 1 of the present invention; FIG. (a) is a low resolution scanning electron micrograph of MXene nanotubes; FIG. (b) is a high resolution scanning electron micrograph of MXene nanotubes;
FIG. 2 is a TEM image of MXene nanotubes prepared in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of MXene nanotubes prepared in example 2 of the present invention;
FIG. 4 is a scanning electron micrograph of MXene nanotubes prepared in example 3 of the present invention;
FIG. 5 is a SEM photograph of MXene nanotubes prepared in example 4 of the present invention;
fig. 6 is a scanning electron micrograph of MXene nanotubes prepared according to example 5 of the present invention.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has made extensive research and practice to propose the technical solution of the present invention, and further explains the technical solution, the implementation process and the principle, etc. as follows. It is to be understood, however, that within the scope of the present invention, each of the above-described features of the present invention and each of the features described in detail below (examples) may be combined with each other to form new or preferred embodiments.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
(1) MXene was dispersed in N, N-dimethylformamide at room temperature under normal pressure to prepare 4ml of 10mgmL-1The dispersion of (4).
(2) Dissolving polyacrylonitrile into the MXene dispersion liquid prepared in the step (1) at the temperature of 50 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 100mg mL-1。
(3) Dissolving polymethyl methacrylate in N, N-dimethylformamide at 60 deg.C to obtain 200mg mL-1A homogeneous solution.
(4) And (3) filling the mixed solution obtained in the step (2) into an injector A, filling the solution obtained in the step (3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine. The mixed solution in the step (2) is an outer layer solution, and the propelling speed is 1.0mlh-1The solution in the step (3) is inner layer solution, and the advancing speed is 0.8ml h-1The voltage of the positive electrode is 18kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 15cm, and a rotating metal roller is used as a collecting device.
(5) By using tube furnace pairsAnd (4) annealing the material collected in the step (4), wherein the treatment temperature is 600 ℃, the treatment time is 1h, and the MXene nanotube is obtained after treatment. As shown in FIG. 1, MXene nanotubes have a tube diameter of 0.5 μm and a wall thickness of 0.02. mu.m. The structural formula of the MXene nanotube is Ti3C2。
Example 2
(1) MXene was dispersed in N, N-dimethylformamide at room temperature under normal pressure to prepare 4ml of a solution having a concentration of 40mgmL-1The dispersion of (4).
(2) Dissolving polyacrylonitrile into the MXene dispersion liquid prepared in the step (1) at the temperature of 55 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 110mg mL-1。
(3) The polymethyl methacrylate was dissolved in N, N-dimethylformamide at 70 ℃ to give a solution having a concentration of 225mg mL-1A homogeneous solution.
(4) And (3) filling the mixed solution obtained in the step (2) into an injector A, filling the solution obtained in the step (3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine. The mixed solution in the step (2) is an outer layer solution, and the propelling speed is 1.1mlh-1The solution in the step (3) is inner layer solution, and the advancing speed is 0.9ml h-1The voltage of the positive electrode is 20kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 16cm, and a rotating metal roller is used as a collecting device.
(5) And (4) annealing the material collected in the step (4) by using a tube furnace, wherein the treatment temperature is 650 ℃, the treatment time is 1.5h, and the MXene nano tube is obtained after treatment. As shown in FIG. 3, the tube diameter of MXene nanotubes was 0.8 μm and the wall thickness was 0.05. mu.m. The structural formula of the MXene nanotube is Nb4C3。
Example 3
(1) MXene is dispersed in N, N-dimethylformamide under normal temperature and pressure to prepare 4ml of solution with the concentration of 60mgmL-1The dispersion of (4).
(2) Dissolving polyacrylonitrile into the MXene dispersion liquid prepared in the step (1) at the temperature of 60 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 120mg mL-1。
(3) Dissolving polymethyl methacrylate in N, N-dimethylformamide at 75 deg.C to obtain 250mg mL-1A homogeneous solution.
(4) And (3) filling the mixed solution obtained in the step (2) into an injector A, filling the solution obtained in the step (3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine. The mixed solution in the step (2) is an outer layer solution, and the propelling speed is 1.2mlh-1The solution in the step (3) is an inner layer solution, and the propelling speed is 1.0ml h-1The voltage of the positive electrode is 22kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 18cm, and a rotating metal roller is used as a collecting device.
(5) And (4) annealing the material collected in the step (4) by using a tube furnace, wherein the treatment temperature is 700 ℃, the treatment time is 2 hours, and the MXene nanotube is obtained after treatment. As shown in FIG. 4, the tube diameter of MXene nanotubes was 1 μm, and the wall thickness was 0.08. mu.m. The structural formula of the MXene nanotube is Mo2V3C2。
Example 4
(1) MXene was dispersed in N, N-dimethylformamide at room temperature under normal pressure to prepare 4ml of a solution having a concentration of 40mgmL-1The dispersion of (4).
(2) Dissolving polyacrylonitrile into the MXene dispersion liquid prepared in the step 1) at the temperature of 50 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 120mg mL-1。
(3) At 70 ℃, the polystyrene is dissolved in N, N-dimethylformamide to form a concentration of 200mg mL-1A homogeneous solution.
(4) And (3) filling the mixed solution obtained in the step (2) into an injector A, filling the solution obtained in the step (3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine. The mixed solution in the step (2) is an outer layer solution, and the propelling speed is 1.2mlh-1The solution in the step (3) is inner layer solution, and the advancing speed is 0.9ml h-1The voltage of the positive electrode is 20kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 16cm, and a rotating metal roller is used as a collecting device.
(5) Using a tube furnace pair(4) The MXene nano tube is obtained after the annealing treatment of the collected material at the temperature of 650 ℃ for 2 h. As shown in FIG. 5, the tube diameter and wall thickness of MXene nanotubes were 0.6 μm and 0.1. mu.m, respectively. The structural formula of the MXene nanotube is V4C2N。
Example 5
(1) MXene was dispersed in N, N-dimethylformamide at room temperature under normal pressure to prepare 4ml of a solution having a concentration of 40mgmL-1The dispersion of (4).
(2) Dissolving polyacrylonitrile into the MXene dispersion liquid prepared in the step 1) at the temperature of 55 ℃, and uniformly mixing, wherein the concentration of the polyacrylonitrile in the mixed solution is 120mg mL-1。
(3) Dissolving polyvinylpyrrolidone in N, N-dimethylformamide at 70 deg.C to obtain a solution with a concentration of 200mg mL-1A homogeneous solution.
(4) And (3) filling the mixed solution obtained in the step (2) into an injector A, filling the solution obtained in the step (3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine. The mixed solution in the step (2) is an outer layer solution, and the propelling speed is 1.0mlh-1The solution in the step (3) is inner layer solution, and the advancing speed is 0.8ml h-1The voltage of the positive electrode is 18kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 16cm, and a rotating metal roller is used as a collecting device.
(5) And (4) annealing the material collected in the step (4) by using a tube furnace, wherein the treatment temperature is 700 ℃, the treatment time is 2 hours, and the MXene nanotube is obtained after treatment. As shown in FIG. 6, the tube diameter of MXene nanotubes was 1 μm, and the wall thickness was 0.05. mu.m. The structural formula of the MXene nanotube is W4C3。
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. The MXene nanotube is characterized in that the MXene nanotube is formed by axially overlapping two-dimensional MXene sheets in a staggered manner, the outer diameter of the MXene nanotube is 0.5-1 mu M, the wall thickness of the MXene nanotube is 0.02-0.1 mu M, and the structural general formula of the MXene nanotube is Mn+1XnOr (M)1,M2)n+1XnOr Mn+1(X1,X2)nOne or a combination of two or more of them;
said Mn+1XnWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x ═ C, N;
said (M)1,M2)n+1XnIn, M1,M2＝Ti,Nb,V,Mo,Zr,Cr,W,Ta；n＝1,2,3；X＝C,N；
Said Mn+1(X1,X2)nWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x1,X2＝C,N。
2. A general synthesis method of MXene nanotubes as claimed in claim 1, characterized by the following steps:
1) dispersing MXene in N, N-dimethylformamide at normal temperature and pressure to prepare a dispersion liquid;
2) dissolving polyacrylonitrile in the MXene dispersion liquid prepared in the step 1) at the temperature of 50-60 ℃, and uniformly mixing, wherein the concentration of polyacrylonitrile in the mixed solution is 100-120mg mL-1；
3) Dissolving a sacrificial template agent in N, N-dimethylformamide at the temperature of 60-75 ℃ to form a homogeneous solution;
4) loading the mixed solution obtained in the step 2) into an injector A, loading the homogeneous solution obtained in the step 3) into an injector B, and carrying out coaxial electrostatic spinning by using an electrostatic spinning machine; the spinning parameters are as follows: the mixed solution in the step 2) is an outer layer solution, and the propelling speed is 1.0-1.2mlh-1The solution in the step 3) is an inner layer solution, and the advancing speed is 0.8-1.0ml h-1The voltage of the positive electrode is 18-22kv, the voltage of the negative electrode is-2.5 kv, the spinning distance is 15-18cm, and a rotating metal roller is used for collectionA device;
5) annealing the material collected in the step 4) by using a tube furnace to obtain the MXene nanotube.
3. The general synthesis method of MXene nanotubes as claimed in claim 2, wherein the concentration of the dispersion in step 1) is 10-60mg mL-1。
4. The general synthesis method of MXene nanotubes as claimed in claim 2, wherein the sacrificial template in step 3) is one or more of polymethylmethacrylate, polystyrene, and polyvinylpyrrolidone.
5. The general synthesis method of MXene nanotubes as claimed in claim 2, wherein the concentration of the sacrificial template solution in step 3) is 200-250mg mL-1。
6. The general synthesis method of MXene nanotubes as claimed in claim 2, wherein the annealing temperature in step 5) is 600-700 ℃ and the treatment time is 1-2 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114438618A (en) * | 2022-03-08 | 2022-05-06 | 北京化工大学 | Fiber and method for producing the same |
| CN116779208A (en) * | 2022-03-09 | 2023-09-19 | 北京航空航天大学 | Conductive agent, conductive paste, preparation method and application thereof |
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