CN112499601B - Method for efficiently preparing thin layer MXene - Google Patents
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for efficiently preparing a thin layer MXene, which relates to the technical field of MAX materials, and is characterized in that an etched MAX raw material is dispersed in a stripping solution, and after oscillation stripping is performed at room temperature, a few-layer MXene two-dimensional nano-sheet material can be obtained through freeze drying. The novel stripping material creatively realizes the efficient stripping of the thin layer MXene, improves the yield, greatly reduces the cost and further improves the stability of the MXene.
Description
Technical Field
The invention relates to the technical field of MAX materials, in particular to a preparation method of MXene.
Background
MXene as one new kind of two-dimensional (2D) transition metal nanometer material with the chemical expression of M n+1 X n (M is a transition metal element, X is carbon or nitrogen element, n=1, 2, 3). The MXene material has excellent conductivity, and the surface of the MXene material contains a large amount of functional groups (-F, -OH, -O), so that the MXene material also has good hydrophilicity. Because of these unique physicochemical properties, MXene has been widely used in the fields of catalysis, energy storage, sensors, water treatment, and the like since 2011.
The conventional preparation methods of MXene at present comprise an acid etching method (hydrofluoric acid or corresponding fluoride salt), an alkali etching method, a high-temperature molten salt method and the like. And etching the A layer element (Al, si and the like) in the raw material MAX by adopting a proper etchant, and then obtaining the two-dimensional thin layer MXene nano sheet layer by oscillation stripping. However, in the preparation process, the simple oscillation is difficult to effectively and completely peel off the nano-sheets, and meanwhile, the peeled two-dimensional nano-sheets are extremely easy to irreversibly stack and agglomerate under the action of Van der Waals force, so that the yield of the thin layer MXene is extremely low, the cost is high, and the thin layer MXene cannot be applied commercially.
Disclosure of Invention
Based on the problem of low yield of the thin layer MXene, the invention aims to provide a method for efficiently preparing the thin layer MXene material so as to overcome the defects in the prior art.
It is a further object of the invention to provide the use of a thin layer of MXene two-dimensional material.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a method for efficiently preparing a thin layer MXene comprises the following specific processes: and dispersing the MAX block material of which the A layer elements (Al, si and the like) are etched into a certain amount of stripping solution, and performing oscillation stripping and freeze drying to obtain the thin-layer MXene two-dimensional material with high yield.
Furthermore, the stripping solution of the method for efficiently preparing the thin layer MXene is an aqueous solution comprising carbon nano tubes, chitosan and polyacrylamide.
Further, the method for efficiently preparing the thin layer MXene has the concentration of stripping solution of 0.01-100mg/mL.
Further, in the method for efficiently preparing the thin layer MXene, the mass ratio of the added stripping material to the MAX material to be stripped is 1-100%. The optimal proportion is 2% -20%.
Furthermore, the oscillation time of the method for efficiently preparing the thin layer MXene is 0.1h-10h.
Further, the method for efficiently preparing the thin layer MXene has the thickness of 1.5-100nm and the structural size of 0.1-10 mu m.
In another aspect of the invention, there is provided the use of a thin layer of MXene two-dimensional material in the preparation of an energy storage material, a composite nanomaterial, a lubricating material, an adsorbing material or a catalyst.
Compared with the prior art, the invention has the following advantages:
(1) The invention provides a method for efficiently preparing a thin layer MXene, which is based on the principle that bulk MAX is efficiently stripped by utilizing the rheological property and viscosity of stripping materials to obtain a thin layer MXene two-dimensional nano sheet material.
(2) The method for efficiently preparing the thin layer MXene provided by the invention creatively uses the novel stripping material, and the stripping material has the advantages of wide sources, easiness in obtaining and low cost, and can greatly reduce the preparation cost of the thin layer MXene two-dimensional nano sheet material.
(3) According to the method for efficiently preparing the thin layer MXene, the surface groups (amino, hydroxyl and the like) of the stripping material can coordinate with metal atoms on the surface of the MXene, so that transition atoms are prevented from being oxidized, and the stability of the MXene is further improved.
(4) The method for efficiently preparing the thin layer MXene has the advantages of mild reaction conditions, simple operation and environmental friendliness, can realize high yield, is beneficial to large-scale production, and improves the application prospect of MXene.
(5) The novel stripping material is creatively used, and the rheological property and lubricity of the stripping material enable the electrical property, dielectric property and the like of the prepared thin-layer MXene two-dimensional nano sheet material to be adjustable, so that the stripping material has a good application prospect in the fields of energy storage, composite materials, lubricating materials, adsorption materials, catalysts and the like.
Drawings
FIG. 1 is an SEM photograph of a two-dimensional nano-sheet (b, c, d) based on the MXene precipitate (a) and the exfoliated thin layer MXene in example 1, which were not exfoliated by the conventional method.
FIG. 2 is an X-ray diffraction (XRD) spectrum based on the thin-layer MXene two-dimensional nanoplatelets of example 1 and the MXene precipitates that were not exfoliated by conventional methods.
Fig. 3 is an SEM photograph based on the thin-layer MXene two-dimensional nanoplatelets (a, b) and MXene precipitates (c, d) that were not exfoliated using the conventional method in example 2.
FIG. 4 is an X-ray diffraction (XRD) spectrum based on the thin-layer MXene two-dimensional nanoplatelets of example 2 and the MXene precipitates that were not exfoliated by conventional methods.
FIG. 5 is an SEM photograph of an unpeeled MXene precipitate (a) and a exfoliated thin layer of MXene two-dimensional nanoplatelets (b, c, d) based on the conventional method in example 3.
FIG. 6 is an X-ray diffraction (XRD) spectrum based on the thin-layer MXene two-dimensional nanoplatelets of example 3 and the MXene precipitates that were not exfoliated by conventional methods.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the inventive concepts pertain. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and put forward a technical solution of the present invention, and the technical solution, the implementation process and principle thereof will be further explained as follows.
Briefly, the present invention is a method for efficiently preparing a thin layer of MXene: dispersing the etched MAX raw material in stripping solution, oscillating and stripping at room temperature, and freeze-drying to obtain the thin-layer MXene two-dimensional nano-sheet material.
The inventors of the present invention have made an inventive effort and the resulting solution has made a significant improvement over the prior art in terms of reducing production costs, increasing reaction yields and improving reaction results, all of which are of significant positive significance. The specific explanation is as follows:
the method for efficiently preparing the thin layer MXene creatively uses the novel stripping material, realizes the efficient stripping of the thin layer MXene, improves the yield, greatly reduces the cost and further improves the stability of the MXene.
Compared with the prior art, the method has the advantages that the etched MAX nano sheet layer is stripped by repeated oscillation in water, ethanol or the like, the energy consumption is high, and the yield is low (10% -20%). The invention creatively adopts the novel stripping material and utilizes the rheological property and viscosity of the novel material to strip the etched MAX effectively. The stripping process is as follows: in the oscillation process, the novel stripping material can effectively reduce Van der Waals force between MXene two-dimensional nano sheets, and meanwhile, the self viscosity of the material generates larger tearing force in the oscillation process, so that MAX is stripped efficiently. In particular, polar groups (amino, hydroxyl) on the surface of the material can coordinate with transition metal atoms on the surface of MXene, thereby improving the stability of MXene.
Furthermore, the novel stripping material is creatively used for preparing the thin-layer MXene two-dimensional material, the chemical stability and the thermal stability of the thin-layer MXene two-dimensional material are superior to those of the traditional MXene two-dimensional nano-sheet, and the thin-layer MXene two-dimensional material has more abundant adjustable spaces for electrical properties, dielectric constants and the like.
The invention will be described in detail with reference to the following examples and drawings.
Embodiment one:
adding 2g of lithium fluoride into 40ml of 9M hydrochloric acid, and uniformly mixing; then, MAX having a mass of 2g was slowly added to the obtained mixed solution, and the mixed solution was stirred at 35℃for 24 hours. And then centrifugally washing to neutrality to obtain the etched MAX raw material.
1g of etched MAX raw material is weighed and dispersed in 15ml of 0.6mg/ml carbon nano tube aqueous solution, and after shaking and stripping for 1h, the thin-layer MXene two-dimensional nano material can be obtained through freeze drying. For comparison, 1g of the etched MAX raw material was weighed and dispersed in 15ml of an aqueous solution, and after shaking and peeling for 1 hour, the MXene precipitate was obtained by freeze-drying.
FIG. 1 is an SEM photograph of an unpeeled MXene precipitate (a) and an efficiently exfoliated MXene (b, c, d) using an aqueous carbon nanotube solution in example 1. As shown in the figure, the thin layer MXene peeled by the carbon nano tube aqueous solution presents a loose two-dimensional nano lamellar structure, the lamellar layer is ultrathin, and the lamellar thickness of a single layer is about 10nm. While the comparative MXene precipitate exhibited a largely massive structure.
FIG. 2 is an X-ray diffraction (XRD) spectrum based on the thin-layer MXene two-dimensional nanoplatelets and MXene precipitates of example 1. As shown, a distinct peak (5) was observed for the exfoliated MXene two-dimensional material, indicating that the interlayer spacing of the MXene was increased. Embodiment two:
and weighing 1g of etched MAX raw material, dispersing in 20ml of 5mg/ml chitosan aqueous solution, oscillating and stripping for 1h, and freeze-drying to obtain the MXene two-dimensional nanosheet material. For comparison, 1g of the etched MAX raw material was weighed and dispersed in 20ml of an aqueous solution, and after shaking and peeling for 1 hour, the MXene precipitate was obtained by freeze-drying.
FIG. 3 is an SEM photograph of two-dimensional nanoplatelets (a, b) and precipitants (c, d) of MXene based on the thin layer of MXene in example 2. As shown in the figure, the thin layer MXene peeled by the chitosan aqueous solution presents loose two-dimensional nano lamellar structure lamellar ultrathin, and the lamellar thickness of a single layer is about 10nm. While the MXene precipitate mostly exhibits a thick, massive structure.
FIG. 4 is an X-ray diffraction (XRD) spectrum based on the thin-layer MXene two-dimensional nanoplatelets and MXene precipitates of example 2. As shown in the figure, after stripping, unlike the MXene precipitate, the diffraction peak of the highly efficient stripped thin layer MXene disappeared, indicating that the bulk structure of MAX after etching was well stripped.
Example III
And weighing 0.5g of etched MAX raw material, dispersing in 5ml of 5mg/ml polyacrylamide aqueous solution, oscillating and stripping for 1h, and freeze-drying to obtain the thin-layer MXene two-dimensional nanomaterial. For comparison, 0.5g of the etched MAX raw material is weighed and dispersed in 5ml of water solution, and after shaking and stripping for 1h, the MXene precipitate is obtained by freeze drying.
Fig. 5 is an SEM photograph based on the MXene precipitate (a) and the exfoliated thin layers MXene (b, c, d) in example 3. As shown in the figure, the thin layer MXene peeled by the Polyacrylamide (PAM) aqueous solution presents a loose two-dimensional nano lamellar structure, the lamellar layer is ultrathin, and the lamellar thickness of a single layer is about 10nm. While the MXene precipitate mostly exhibits a thick, massive structure.
FIG. 6 is an X-ray diffraction (XRD) spectrum of a thin layer of MXene two-dimensional nanoplatelets and MXene precipitates based on example 3. As can be seen from the comparison, the etched MAX material is well stripped.
Claims (3)
1. A method of preparing a thin layer of MXene, characterized by: dispersing the MAX block material of which the element of the layer A is etched into a certain amount of stripping solution, and obtaining a thin-layer MXene two-dimensional nano-sheet material after oscillation stripping; wherein:
the element of the layer A is Al or Si;
the oscillation time is 0.1h-10h;
the stripping solution is an aqueous solution of chitosan or polyacrylamide, the concentration is 0.01-100mg/mL, and the mass ratio of the added stripping material to the MAX material to be stripped is 1-100%;
the thickness of the thin MXene two-dimensional nano lamellar material is 1.5-100nm, and the lamellar structure size is 0.1-10 mu m.
2. The method for preparing a thin layer of MXene according to claim 1, characterized in that: the mass ratio of the added stripping material to the MAX material to be stripped is 2% -20%.
3. Use of the thin-layer MXene two-dimensional nanosheet material prepared by the method of claim 1 or 2 for the preparation of energy storage materials, composite nanomaterials, lubricating materials, adsorption materials or catalysts.
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| CN114011261B (en) * | 2021-10-28 | 2022-09-06 | 大连理工大学 | General method for enhancing stability of MXene aqueous solution |
| CN114989875B (en) * | 2022-06-21 | 2023-01-31 | 中国科学院兰州化学物理研究所 | Application of MXene solvent-free nano fluid in tribology field |
| CN115353108A (en) * | 2022-08-23 | 2022-11-18 | 太原理工大学 | Preparation method of large-size MXene nanosheet |
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