CN114956178A - Electrochemical stripping method of two-dimensional layered material - Google Patents
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Abstract
The invention discloses an electrochemical stripping method of a two-dimensional layered material, which is characterized by comprising the following steps: adding a two-dimensional layered material to a composition containing PF 6 Uniformly mixing the organic salt solution, performing polarization treatment by adopting a two-electrode system, and purifying to obtain a stripped two-dimensional nanosheet; said PF containing 6 The solvent of the organic salt solution of (a) is dimethyl sulfoxide and/or N-methylpyrrolidone. The electrochemical stripping method provided by the invention does not need the tedious steps of fixing the two-dimensional layered raw material on the surface of the electrode and repeatedly operating to increase the yield of the two-dimensional nanosheets, avoids the defect that the yield is obviously reduced due to the fact that bubbles drive the non-stripped particles to fall off from the surface of the electrode, can drive the two-dimensional layered material particles to be directly, rapidly and continuously stripped, and realizes simple, large-scale and high-yield preparation of the thin-layer two-dimensional material.
Description
Technical Field
The application belongs to the technical field of two-dimensional material preparation, and particularly relates to an electrochemical stripping method of a two-dimensional layered material.
Background
As a typical transition metal sulfide, the atomic structure of molybdenum disulfide is formed by covalently linking two sulfur atoms on both sides with a molybdenum atom in the middle, and the plane of the molybdenum disulfide can be continuously extended to present a two-dimensional planar morphology. The single-layer molybdenum disulfide has the thickness of about 0.65nm, has intrinsic semiconductor characteristics, and has remarkable application prospects in the fields of electrocatalysis, electrochemical sensing, electronic devices and the like. Research shows that the physical and chemical properties of molybdenum disulfide are closely related to the number of layers, such as band gap, specific surface area and lithium storage capacity, but the molybdenum disulfide often has particle morphology with close packing and random size and number of layers due to van der waals attractive force between the layers, which limits large-area processing and intrinsic property research of the molybdenum disulfide. Therefore, scientists are always exploring different layered material stripping methods, expecting to realize the fast, high-yield and nondestructive preparation of thin layer or even single layer molybdenum disulfide, and laying a foundation for intrinsic characteristic exploration, controllable processing and large-scale industrial application.
The overlooking and cross-section chemical structures of the molybdenum disulfide are respectively shown as a formula (I) and a formula (II), and the molybdenum disulfide is a sandwich structure consisting of two layers of sulfur atoms and a middle layer of molybdenum atoms. The lamellar molybdenum disulfide was observed microscopically to be in the form of a block, which was formed by the stacking of the layers of molybdenum disulfide due to van der Waals interactions.
With the continuous and deep research, molybdenum disulfide has excellent performance in the fields of sensing, electrocatalysis, energy conversion and the like. In addition, studies have reported that the bandgap of molybdenum disulfide exhibits a tendency to decrease with increasing number of layers, and reference may be made to studies in phys. In order to explore the intrinsic properties of several layers or even a single layer of molybdenum disulfide, researchers have developed various methods for preparing ultrathin molybdenum disulfide, such as chemical vapor deposition, molecular beam epitaxy, and the like. However, these methods have the disadvantages of complicated operation and harsh synthesis conditions, and it is difficult to obtain a small layer of molybdenum disulfide on a large scale. Therefore, it is necessary to develop a simple, efficient and nondestructive stripping method for molybdenum disulfide, and the electrochemical stripping method provides a new approach to this requirement.
Among various methods for preparing two-dimensional materials, electrochemical stripping, which is a typical strategy from top to bottom, has the advantages of high quality and rapidness. To date, the working mechanisms of common electrochemical stripping are mainly the following two: firstly, charged substances are inserted between layers or ions with the same charge in the layers are exchanged, so that the interlayer spacing can be increased, and the interlayer mutual attraction and the energy required by stripping are reduced; and secondly, the bubbles drive interlayer expansion, and electroactive substances inserted between the layers can exchange electrons with the electrodes of the layered materials to generate bubbles so as to drive interlayer expansion and thin layer peeling. Electrochemical exfoliation has been successfully applied to obtain few-layer flakes of various layered materials, such as molybdenum disulfide, graphene, black phosphorus, carbon and nitrogen compounds, and the like. However, the above-mentioned conventional electrochemical peeling method has a problem that when a layered raw material is used as an electrode, it is difficult to avoid a problem that particles fall off from the surface of the electrode to decrease the yield, and it is difficult to fix a layered raw material having a size of mm or less.
Disclosure of Invention
In order to solve the problems, the invention provides an electrochemical stripping method of a two-dimensional layered material, which can realize direct, rapid and continuous stripping of the two-dimensional layered material.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
an electrochemical stripping method for two-dimensional laminar material includes adding two-dimensional laminar material to the material containing PF 6 - Uniformly mixing the organic salt solution, adopting a two-electrode system to carry out polarization treatment, and purifying to obtain stripped two-dimensional nanosheets; said PF containing 6 - The solvent of the organic salt solution of (a) is dimethyl sulfoxide and/or N-methylpyrrolidone.
According to the invention, the two-dimensional layered material is selected from one of molybdenum disulfide, tungsten diselenide, boron nitride and graphite-like phase carbon nitride.
According to the invention, the PF-containing 6 - The organic salt solution of (A) is PF-containing 6 - Preferably containing PF 6 - An organic solution of a propyl ammonium salt or a butyl ammonium salt.
According to the invention, the two-dimensional layered material and the article containing PF 6 - The mass ratio of the organic salt of (1): (30-120), preferably 1: (40-80).
According to the invention, the PF-containing 6 - The concentration of the organic salt solution of (3) is in the range of 0.01 to 1mol/L, preferably 0.05 to 0.5 mol/L.
According to the invention, in the two-electrode system, a conductive cylindrical concave pool is selected as a container and used as a cathode, and the material is glassy carbon or stainless steel.
According to the invention, in the two-electrode system, a platinum wire is selected as an anode.
According to the invention, the temperature of the polarization treatment is between 0 and 30 ℃, preferably between 15 and 25 ℃.
According to the invention, the time of the polarization treatment is 10-120min, preferably 20-90min, and more preferably 30-60 min.
According to the present invention, the voltage of the polarization treatment is 1 to 30V, preferably 5 to 20V, and more preferably 8 to 12V.
According to the invention, the purification process specifically comprises: and (3) carrying out suction filtration, washing and drying on the product after polarization treatment, dispersing in an organic solvent, centrifuging to obtain a supernatant, and drying to obtain the stripped two-dimensional nanosheet.
The organic solvent is selected from dimethyl sulfoxide, N-dimethylformamide or N-methylpyrrolidone, and is preferably N, N-dimethylformamide.
The method is based on single-particle collision electrochemical reaction, can provide sufficient electrochemical collision interfaces for particles in a solution and dynamic constants related to rapid electrochemical reaction, does not need to fix the two-dimensional layered raw materials on the surface of the electrode and repeat operation to increase the yield of the two-dimensional nanosheets, avoids the defect that the yield is remarkably reduced due to the fact that bubbles drive unpeeled particles to fall off from the surface of the electrode, can drive the direct, rapid and continuous stripping of the two-dimensional layered material particles, and realizes the simple, large-scale and high-yield preparation of the thin-layer two-dimensional material.
The invention has the advantages that:
1. the electrochemical stripping method provided by the invention does not need the tedious steps of fixing the two-dimensional layered raw material on the surface of the electrode and repeatedly operating to increase the yield of the two-dimensional nanosheets, avoids the defect that the yield is obviously reduced due to the fact that bubbles drive the non-stripped particles to fall off from the surface of the electrode, can drive the two-dimensional layered material particles to be directly, rapidly and continuously stripped, and realizes simple, large-scale and high-yield preparation of the thin-layer two-dimensional material.
2. The electrochemical stripping method is proved by a series of characterization results of Raman spectrum, infrared spectrum, photoelectron spectrum and high-resolution transmission electron microscope, is based on non-covalent acting force, and does not introduce any defect into a two-dimensional material structure.
3. The electrochemical stripping method of the invention is based on a specific electrochemical system and contains PF 6 - The organic salt and the solvent (dimethyl sulfoxide and/or N-methyl pyrrolidone) directly strip the two-dimensional layered material through the electrochemical reaction in which the organic salt and the solvent participate, and the method is simple and efficient.
Drawings
Figure 1 is an optical microscope image of molybdenum disulfide powder.
Fig. 2 is a picture (a) of the apparatus for electrochemical stripping reaction and a picture (b) of the N, N-dimethylformamide dispersion of molybdenum disulfide before (left) and after (right) stripping in example 1.
FIG. 3 is an eMOS in example 1 2 A transmission electron microscope image (a) and an atomic force microscope image (b) of the nanosheet; eMOS 2 The number of layers (c) and the size (d) of (c) are counted.
FIG. 4 is eMOS in example 1 2 The high-resolution transmission electron microscope image (a) and the corresponding selected electron diffraction image (b); molybdenum disulfide before electrochemical stripping (MoS) 2 Feedstock) post (eMoS) 2 ) The Raman spectrum (c) and the photoelectron spectrum (d) of (A).
Fig. 5 shows a picture (a) and a transmission electron microscope image (b) of the N, N-dimethylformamide dispersion liquid of the tungsten disulfide in example 2 after peeling.
Fig. 6 shows a picture (a) and a transmission electron microscope image (b) of the N, N-dimethylformamide dispersion liquid of tungsten diselenide in example 3 after being peeled off.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. The following examples are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
In the following examples, raw materials such as molybdenum disulfide, tungsten diselenide and the like can be obtained from commercial sources, and are conventional medicines, and the purity is analytically pure. As can be seen from fig. 1, the molybdenum disulfide powder was accumulated by the pi-pi interaction between layers and was in the form of bulk powder.
Example 1
1.1 electrochemical stripping Process for molybdenum disulfide powder
100mg of molybdenum disulfide powder was mixed with 20mL of a dimethyl sulfoxide solution having a concentration of 0.5M tetrabutylammonium hexafluorophosphate, and transferred to a conductive glassy carbon cell as a cathode and a platinum wire as an anode, as shown in FIG. 2 (a). Applying a potential difference of 10V, stirring at normal temperature and normal pressure, reacting for 1 hour, observing continuous fine bubbles at the edge of the tank wall during the reaction, and obtaining uniform black colloid after the reaction is finished.
1.2 thin stripping of molybdenum disulfide (eMOS) 2 ) Purification of (2)
Filtering the black colloid, removing residual organic salt and by-products by using acetone, and drying in vacuum to obtain fluffy solid MoS 2 . Ultrasonically dispersing the strain in N, N-dimethylformamide, centrifuging (2000 rpm) for 10 minutes, and taking yellow-green supernatant, namely the thin-layer product eMOS 2 The dispersion of (4). The product was dried and weighed, resulting in a yield of about 70 wt%. Diluted eMOS 2 The dispersion showed a significant tyndall effect upon irradiation with laser light, as shown in fig. 2 (b).
1.3、eMoS 2 The appearance characterization and the analysis of thickness and size
eMOS (enhanced multimedia over silicon) 2 The dispersion liquid is dripped on the surface of the copper grid and dried, and the transmission electron microscope characterization result proves that the ultrathin eMOS obtained by the method 2 And the organic salts and by-products have been removed by washing, as shown in fig. 3 (a).
eMOS (enhanced multimedia over silicon) 2 The dispersed liquid is dripped on the surface of a silicon wafer and dried, and the characterization result of an atomic force microscope proves that the prepared eMOS 2 In a few layers or even in a single layer. Prepared eMOS 2 About 80% of the thickness is 1-5 layers, 19% of which is a single layer, as shown in fig. 3 (b-c). eMOS 2 The lateral dimensions of (A) are distributed in a large amount of about 10 μm as shown in FIG. 3 (d). The results directly prove that the method successfully realizes the high-efficiency stripping of the molybdenum disulfide and lays a foundation for researching the intrinsic properties of a single layer or a few layers of molybdenum disulfide in the future.
1.4、eMoS 2 Structural and elemental characterization of
eMOS (enhanced multimedia over silicon) 2 The dispersed liquid is dripped on the surface of the copper grid and dried, and the structure of the copper grid is represented by a high-resolution transmission electron microscope and selected electron diffraction, eMOS 2 The lattice constant in the (100) plane was 0.28nm, which is consistent with the results for the molybdenum disulfide powder, as shown in figure 4 (a). In addition, the bright spots in the selected area electron diffraction image are proved to be distributed in a hexagon, which shows that the eMOS is applied to the surface of the substrate 2 Has high crystallinity, as shown in FIG. 4 (b). These results demonstrate that eMoS prepared by this method 2 Structural defects are not introduced, and the original high crystallinity of the molybdenum disulfide is still maintained.
eMOS (enhanced multimedia over silicon) 2 The dispersion liquid is dripped on the surface of the silicon chip and dried, and the Raman spectrum result shows that the characteristic vibration peaks of the molybdenum disulfide before and after stripping are almost consistent, which indicates that the method is used for destroying the structure of the molybdenum disulfide. Then, its elemental composition, eMOS, was characterized by photoelectron spectroscopy 2 Consisting essentially of molybdenum (Mo) and sulfur (S), wherein oxygen (O) may originate from oxygen adsorption or a small amount of oxygen-containing functional groups, was nearly identical to the characterization results for molybdenum disulfide particles, as shown in fig. 4(d), illustrating eMoS prepared by the methods of the present application 2 Without introduction of other elements or functional groups, eMOS 2 The elemental composition before stripping is maintained.
Example 2
100mg of tungsten disulfide powder was mixed with 20mL of a 0.5M solution of tetrabutylammonium hexafluorophosphate in dimethyl sulfoxide, and transferred to a conductive glassy carbon cell, which served as the cathode and a platinum wire as the anode. Applying a potential difference of 10V, stirring at normal temperature and normal pressure, reacting for 1 hour, observing continuous fine bubbles at the edge of the tank wall during the reaction, and obtaining uniform black colloid after the reaction is finished. Purifying and centrifuging to obtain yellow transparent supernatant as thin layer product eWS 2 The dispersion of (4). Diluted WS 2 The dispersion showed a significant tyndall effect upon irradiation with laser light, as shown in fig. 5 (a). Transmission electron microscope characterization results prove that the method obtains the ultrathin WS 2, As shown in fig. 5 (b).
Example 3
100mg of tungsten diselenide powder was mixed with 20mL of a 0.5M solution of tetrabutylammonium hexafluorophosphate in dimethyl sulfoxide, and transferred to a conductive glassy carbon cell, which served as the cathode and a platinum wire as the anode. Applying a potential difference of 10V, stirring and reacting for 1 hour at normal temperature and normal pressure, wherein continuous fine bubbles can be observed at the edge of the tank wall, and uniform black colloid is obtained after the reaction is finished. Purifying and centrifuging to obtain light yellow supernatant, namely the thin-layer product eWSe 2 The dispersion of (4). Diluted WSe 2 The dispersion showed a significant tyndall effect upon irradiation with laser light, as shown in fig. 6 (a). Transmission electron microscope characterization results prove that the method obtains ultrathin WSe 2, As shown in fig. 6 (b).
Comparative example 1
100mg of molybdenum disulfide powder was mixed with 20mL of a 0.5M solution of tetrabutylammonium hexafluorophosphate in dimethyl sulfoxide and transferred to a conductive glass carbon bath. Stirring at normal temperature and pressure for 1 hour without applying a potential difference. After the reaction was completed, the mixture was purified and centrifuged, and the supernatant was found to be almost colorless and the bottom precipitate was still powdery, indicating that molybdenum disulfide could not be peeled off by merely stirring treatment without the participation of electrochemical polarization.
Comparative example 2
100mg of molybdenum disulfide powder was mixed with 20mL of PF-free solution 6 - The pure dimethyl sulfoxide solvent of the organic salt is mixed and transferred into a conductive glassy carbon pool, the glassy carbon pool is used as a cathode, and a platinum wire is used as an anode. A potential difference of 10V was applied, and the mixture was stirred and reacted at normal temperature and pressure for 1 hour. After the reaction was completed, the dispersion was purified and centrifuged, and it was found that the supernatant was almost colorless and the bottom precipitate was still powdery, which is shown in the case where no PF was contained 6 - In the presence of the organic salt, the electrochemical treatment does not strip the molybdenum disulfide.
Comparative example 3
Besides two solvents of dimethyl sulfoxide and N-methyl pyrrolidone, the influence of other 4 polar solvents on electrochemical stripping is examined, wherein the other 4 polar solvents comprise N, N-dimethylformamide, acetonitrile, propylene carbonate and deionized water. Design 4 sets of experiments, respectively mixing 100mg of tungsten diselenide powder with 20mL of the above four solvents with a concentration of 0.5M tetrabutylammonium hexafluorophosphate, transferring the mixture into a conductive glassy carbon pool, wherein the glassy carbon pool is used as a cathode and a platinum wire is used as an anode. Applying a potential difference of 10V, stirring and reacting for 1 hour at normal temperature and pressure, wherein continuous bubbles can be observed at the edge of the cell wall. After the reaction, the dispersion was purified and centrifuged, and the supernatant was found to be almost colorless and the bottom precipitate was still powdery, indicating that molybdenum disulfide could not be stripped from the four solvents selected above.
Claims (10)
1. An electrochemical stripping method of a two-dimensional layered material is characterized in that: adding a two-dimensional layered material to a composition containing PF 6 - Uniformly mixing the organic salt solution, adopting a two-electrode system to carry out polarization treatment, and purifying to obtain stripped two-dimensional nanosheets; said PF containing 6 - The solvent of the organic salt solution of (a) is dimethyl sulfoxide and/or N-methylpyrrolidone.
2. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the two-dimensional layered material is selected from one of molybdenum disulfide, tungsten diselenide, boron nitride and graphite-like phase carbon nitride.
3. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the PF containing 6 - The organic salt solution of (A) is PF-containing 6 - Ammonium salt solution of (1).
4. The electrochemical peeling method of two-dimensional layered material as claimed in claim 3, wherein: the PF containing 6 - The ammonium salt solution of (A) is PF-containing 6 - Or a butylammonium salt.
5. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the two-dimensional layered material and the composition containing PF 6 - The mass ratio of the organic salt of (a) is 1: (30-120).
6. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the PF containing 6 - The concentration of the organic salt solution of (3) is in the range of 0.01 to 1 mol/L.
7. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: in the two-electrode system, a conductive cylindrical concave pool is selected as a container and is used as a cathode, and the material is glassy carbon or stainless steel; platinum wire is selected as anode.
8. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the temperature of the polarization treatment is 0-30 ℃; the time is 10-120 min; the voltage is 1-30V.
9. The electrochemical peeling method of two-dimensional layered material according to claim 1, characterized in that: the purification process specifically comprises: and (3) carrying out suction filtration, washing and drying on the product after polarization treatment, dispersing in an organic solvent, centrifuging to obtain a supernatant, and drying to obtain the stripped two-dimensional nanosheet.
10. The electrochemical peeling method of two-dimensional layered material according to claim 9, characterized in that: the organic solvent is selected from dimethyl sulfoxide, N-dimethylformamide or N-methylpyrrolidone.
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