CN110697778B - Preparation method of tin disulfide molybdenum/tin disulfide nanosheet - Google Patents
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Abstract
The invention discloses a preparation method of a tin disulfide molybdenum/tin disulfide nanosheet. Sn doped MoO3Nanoribbon, SnS2Mixing the nano sheets and thiourea according to a certain proportion, taking water as a solvent, and adding the mixture into a hydrothermal kettle with 25mL of polytetrafluoroethylene as an inner container; heating for tens of hours, and naturally cooling after the reaction is finished; and centrifugally separating a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide planar heterostructure nanosheet. In addition, we also obtained a tin disulfide/molybdenum tin disulfide core-shell structure by adding a surfactant to reduce the surface energy. Sn doped MoO3Nanoribbon, SnS2Mixing the nanosheets, polyvinylpyrrolidone and thiourea according to a certain proportion, adding water serving as a solvent into a hydrothermal kettle with 25mL of polytetrafluoroethylene serving as an inner container; heating for tens of hours, and naturally cooling after the reaction is finished; and centrifugally separating a product obtained by the reaction to obtain the tin disulfide/molybdenum disulfide tin core-shell structure nanosheet.
Description
Technical Field
The invention relates to the field of preparation of heterostructures, in particular to a preparation method of a tin disulfide molybdenum/tin disulfide nanosheet.
Background
In 2004, after graphene was successfully prepared, two-dimensional materials received extensive attention from researchers due to their unique physical and chemical properties and thickness at the atomic level. In a plurality of graphene two-dimensional materials, layered metal disulfides (such as tungsten disulfide, molybdenum disulfide and tin disulfide) have excellent structural, electrical, optical, chemical and thermodynamic properties, so that the layered metal disulfides have great application prospects in the fields of electronics, catalysis, energy conversion, sensing and the like.
The research finds that the properties of the crystal structure, morphology, geometric arrangement, components and the like of the metal disulfide are extremely important for the performance of the electronic device. For example, for some electronic devices, such as gas sensors, the formation of heterojunctions by adjusting the phase state attracts researchers' attention. Currently, 2D heterostructures are mainly prepared by chemical vapor deposition, physical vapor deposition, mechanical transfer and other methods. The practical application range of the heterostructure is limited to a great extent due to the limitation of the preparation method. In contrast, the liquid phase synthesis method enables mass production of heterostructures through a relatively simple experimental apparatus, and the production cost is greatly reduced. However, the liquid phase synthesis method provides low energy and causes defects to be easily generated on the surface of the crystal due to the influence of the solvent and the active agent, thereby resulting in relatively poor crystal quality. In addition, the excellent dispersibility of heterostructures in solution makes them compatible with many device fabrication processes (e.g., drop coating, roll-to-roll printing, and ink jet printing) and widely used in a variety of applications.
However, there was no relevant study of tin disulfide molybdenum/tin disulfide nanoplatelets.
Disclosure of Invention
In order to solve the problem that the performance of a metal disulfide in the prior art needs to be improved, the invention provides a preparation method of a tin disulfide molybdenum/tin disulfide nanosheet, and the surface energy is reduced by adding a surfactant to prepare the tin disulfide/tin disulfide molybdenum core-shell structure nanosheet.
In order to achieve the purpose, the invention adopts the following technical means:
the preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent;
after full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet.
As a further improvement of the invention, the Sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: (3-5).
As a further improvement of the invention, the addition amount of the thiourea is 1-2% of the mass of the water.
As a further improvement of the invention, the hydrothermal reaction is carried out in a hydrothermal kettle with a polytetrafluoroethylene inner container.
As a further improvement of the invention, the hydrothermal reaction is carried out under the condition of heating at 200-220 ℃ for 20-40 hours, and the reaction is naturally cooled after the reaction is finished.
As a further improvement of the invention, the rotation speed of the centrifugal separation is 8000-12000 r/min.
As a further improvement of the invention, the molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
As a further improvement of the invention, a surfactant is also added into the raw materials of the hydrothermal reaction, and the addition amount of the surfactant is 1 to 2 percent of the mass of water.
As a further improvement of the invention, the surfactant is polyvinylpyrrolidone.
As a further improvement of the invention, the molybdenum disulfide tin/tin disulfide nanosheet is of a core-shell structure.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to MoO doped with Sn by a hydrothermal method3Nanoribbon, SnS2The nano-sheet and thiourea are used as raw materials, and the tin disulfide molybdenum/tin disulfide planar heterostructure nano-sheet is prepared under specific reaction conditions. Sn obtained finally0.5Mo0.5S2/SnS2The planar heterostructure is a nanosheet. In addition, SnS is used in the reaction process2Nanosheet as template, Sn produced thereby0.5Mo0.5S2/SnS2The planar heterostructure is also a nanosheet.
Compared with the traditional solid phase and gas phase preparation methods of the heterostructure, the preparation method of the invention can realize the mass production of the heterostructure through a simple experimental device, thereby greatly reducing the production cost.
Further, the surface activity is added to prepare the nanosheets with other structures.
Preferably, the invention also provides disulfide by reducing the surface energy by adding a surfactantA tin/molybdenum disulfide tin core-shell structure. Sn doped MoO3Nanoribbon, SnS2Mixing the nanosheets, polyvinylpyrrolidone and thiourea according to a specific ratio, taking water as a solvent, and carrying out hydrothermal reaction to obtain a product, so as to obtain the tin disulfide/molybdenum disulfide tin core-shell structure nanosheets.
Drawings
FIG. 1 shows Sn in example 10.5Mo0.5S2/SnS2SEM image of planar heterostructure.
FIG. 2 shows Sn in example 10.5Mo0.5S2/SnS2EDX plane scan of planar heterostructure.
FIG. 3 shows Sn in example 10.5Mo0.5S2/SnS2EDX spot analysis plot of planar heterostructure.
FIG. 4 shows Sn in example 10.5Mo0.5S2/SnS2XRD pattern of planar heterostructure.
FIG. 5 shows Sn in example 10.5Mo0.5S2/SnS2XPS plot of planar heterostructure Mo 3 d.
FIG. 6 shows Sn in example 10.5Mo0.5S2/SnS2XPS plot of planar heterostructure Sn 3 d.
FIG. 7 shows Sn in example 10.5Mo0.5S2/SnS2XPS plot of planar heterostructure S2 p.
FIG. 8 shows SnS in example 22/Sn0.5Mo0.5S2SEM image of core-shell structure.
FIG. 9 shows SnS in example 22/Sn0.5Mo0.5S2EDX profile scan of core-shell structure.
FIG. 10 shows SnS in example 22/Sn0.5Mo0.5S2EDX spot analysis of core-shell structures.
FIG. 11 shows SnS in example 22/Sn0.5Mo0.5S2XPS diagram of core-shell Mo 3 d.
FIG. 12 shows SnS in example 22/Sn0.5Mo0.5S2XPS diagram of core-shell structure Sn 3 d.
FIG. 13 shows SnS in example 22/Sn0.5Mo0.5S2XPS plot of core-shell structure S2 p.
Detailed Description
The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent; sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: (3-5), the addition amount of thiourea is 1% -2% of the mass of water, and the hydrothermal reaction is carried out in a hydrothermal kettle with polytetrafluoroethylene as an inner container. The hydrothermal reaction is carried out under the conditions of heating at 200-220 ℃ for 20-40 hours, and the reaction is naturally cooled after the reaction is finished.
After full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet. The rotating speed of centrifugal separation is 8000-12000 r/min. The molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
And the raw materials of the hydrothermal reaction are also added with a surfactant, and the addition amount of the surfactant is 1 to 2 percent of the mass of water. The surfactant is polyvinylpyrrolidone. The molybdenum disulfide tin/tin disulfide nanosheet is of a core-shell structure.
The structure and operation of the present invention will be described in further detail with reference to the following embodiments and the accompanying drawings.
Example 1
Preparation of Sn by hydrothermal method0.5Mo0.5S2/SnS2Planar heterostructure
(1) 3.0mg of Sn-MoO is taken3Nanoribbons, 15mg SnS2Nanosheet, 3.75mmol CS (NH)2)2Adding the mixture and 20mL of deionized water into a hydrothermal kettle with 25mL of polytetrafluoroethylene as an inner container;
(2) putting the mixture into an oven which is heated to 220 ℃ in advance, and heating the mixture for 30 hours at 220 ℃;
(3) after the reaction is finished, naturally cooling the reaction product in a room temperature environment;
(4) centrifugally separating the gray solid obtained by the reaction at the rotating speed of 8000r/min, washing for three times to finally obtain the target product Sn0.5Mo0.5S2/SnS2A planar heterostructure.
For the product Sn in example 10.5Mo0.5S2/SnS2Planar heterostructures were analyzed, as shown in FIG. 1, Sn0.5Mo0.5S2/SnS2SEM image of plane heterostructure, which can illustrate Sn obtained finally0.5Mo0.5S2/SnS2The planar heterostructure is nano-sheet shaped.
As shown in FIG. 2, Sn0.5Mo0.5S2/SnS2In an EDX scan of a planar heterostructure, the content of Mo at the edge portion is much higher than that at the middle portion and the middle portion contains almost no Mo element. In addition, the content of Sn and Mo in the middle part is far higher than that in the edge part, which indicates that SnS is the middle part2And the edge part is Sn0.5Mo0.5S2。
As shown in FIG. 3, Sn0.5Mo0.5S2/SnS2Edge portion Sn of planar heterostructure0.5Mo0.5S2The EDX point analysis chart can show that Mo, Sn, S and Sn are approximately equal to 0.47, 0.53 and 2, so that the nanosheet grown at the edge is Sn0.5Mo0.5S2。
As shown in FIG. 4, Sn0.5Mo0.5S2/SnS2XRD pattern of planar heterostructure with 8.9o and 17.8o corresponding to Sn0.5Mo0.5S2The (001) and (002) planes of the crystal, the other peaks corresponding to SnS2Peak of (2). (PDF card: 23-0677)
As shown in FIG. 5, Sn0.5Mo0.5S2/SnS2XPS plot of Mo 3d in planar heterostructure. XPS of Mo 3d shows that the two peaks corresponding to 1T (228.3 and 231.5eV) have a reduced binding energy of 0.5eV compared to the two peaks corresponding to 2H (228.7 and 232.0 eV). In addition, theAnd the quantitative estimation of the 1T and 2H phase concentration can be realized through the areas corresponding to the peaks of different phase states in the Mo 3d spectrogram. Calculated at Sn0.5Mo0.5S2The concentrations of the 1T crystal phase and the 2H crystal phase were 63% and 37%, respectively.
As shown in FIG. 6, Sn0.5Mo0.5S2/SnS2XPS plot of Sn 3d in planar heterostructure. The peaks at 494.6eV and 486.2eV in the figure correspond to Sn 3 d.
As shown in FIG. 7, Sn0.5Mo0.5S2/SnS2XPS plot of S2 p in planar heterostructure. The peaks at 161.4eV and 162.6eV in the graph correspond to S2-。
Example 2
Hydrothermal method for preparing SnS2/Sn0.5Mo0.5S2Core-shell structure
(1) 3.0mg of Sn-MoO is taken3Nanoribbons, 15mg SnS2Nanosheet, 33mg polyvinylpyrrolidone, 3.75mmol CS (NH)2)2Adding the mixture and 20mL of deionized water into a hydrothermal kettle with 25mL of polytetrafluoroethylene as an inner container;
(2) putting the mixture into an oven which is heated to 220 ℃ in advance, and heating the mixture for 30 hours at 220 ℃;
(3) after the reaction is finished, naturally cooling the reaction product in a room temperature environment;
(4) centrifugally separating the gray solid obtained by the reaction at the rotating speed of 8000r/min, washing for three times to finally obtain the target product SnS2/Sn0.5Mo0.5S2A core-shell structure.
For the product SnS in example 22/Sn0.5Mo0.5S2Core-shell structure analysis, SnS, FIG. 82/Sn0.5Mo0.5S2SEM picture of core-shell structure, and the finally obtained SnS can be illustrated by the SEM picture2/Sn0.5Mo0.5S2The core-shell structure is in a nanometer sheet shape.
As shown in fig. 9, SnS2/Sn0.5Mo0.5S2In an EDX scanning image of the core-shell structure, the content of Mo in the edge part is slightly higher than that in the middle part and the middle partThe part contains almost no Mo element. Furthermore, the method is simple. The content of Sn and Mo in the middle part is far higher than that in the edge part, which indicates that the middle part is SnS2And the edge part is Sn0.5Mo0.5S2。
As shown in fig. 10, SnS2/Sn0.5Mo0.5S2Edge portion Sn of core-shell structure0.5Mo0.5S2The EDX point analysis chart can show that Mo, Sn, S and Sn are approximately equal to 0.56, 0.47 and 2, so that the nanosheet grown at the edge is Sn0.5Mo0.5S2。
As shown in FIG. 11, Sn0.5Mo0.5S2/SnS2XPS plot of Mo 3d in planar heterostructure. XPS of Mo 3d shows that the two peaks corresponding to 1T (228.3 and 231.5eV) have a reduced binding energy of 0.5eV compared to the two peaks corresponding to 2H (228.7 and 232.0 eV). In addition, the quantitative estimation of the 1T and 2H phase concentration can be realized through the corresponding areas of the peaks of different phase states in the Mo 3d spectrogram. Calculated at Sn0.5Mo0.5S2The concentrations of the 1T crystal phase and the 2H crystal phase were 73% and 27%, respectively.
As shown in FIG. 12, Sn0.5Mo0.5S2/SnS2XPS plot of Sn 3d in planar heterostructure. The peaks at 494.6eV and 486.2eV in the figure correspond to Sn 3 d.
As shown in FIG. 13, Sn0.5Mo0.5S2/SnS2XPS plot of S2 p in planar heterostructure. The peaks at 161.4eV and 162.6eV in the graph correspond to S2-。
Example 3
Preparation of Sn by hydrothermal method0.5Mo0.5S2/SnS2Planar heterostructure
The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent; sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: 3, the adding amount of thiourea is 1 percent of the mass of water, and the conditions of the hydrothermal reaction are thatHeating at 200 deg.C for 20 hr, and naturally cooling after reaction.
After full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet. The rotational speed of the centrifugal separation is 8000 r/min. The molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
Example 4
Hydrothermal method for preparing SnS2/Sn0.5Mo0.5S2Core-shell structure
The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent; sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: 5, the adding amount of thiourea is 2 percent of the mass of water, the hydrothermal reaction condition is heating for 40 hours at 220 ℃, and the thiourea is naturally cooled after the reaction is finished.
After full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet. The rotational speed of the centrifugal separation was 12000 r/min. The molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
And (3) adding a surfactant into the raw materials of the hydrothermal reaction, wherein the addition amount of the surfactant is 1% of the mass of water. The surfactant is polyvinylpyrrolidone. The molybdenum disulfide tin/tin disulfide nanosheet is of a core-shell structure.
Example 5
Preparation of Sn by hydrothermal method0.5Mo0.5S2/SnS2Planar heterostructure
The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent; sn doped MoO3Nanobelt andSnS2the mass ratio of the nano sheets is 1: 4, the adding amount of thiourea is 1.5 percent of the mass of water, and the hydrothermal reaction is carried out in a hydrothermal kettle with polytetrafluoroethylene as an inner container. The hydrothermal reaction was carried out under the conditions of heating at 210 ℃ for 30 hours and then cooling naturally after the reaction.
After full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet. The rotation speed of centrifugal separation is 10000 r/min. The molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
Example 6
Hydrothermal method for preparing SnS2/Sn0.5Mo0.5S2Core-shell structure
The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet comprises the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent; sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: 3, the adding amount of thiourea is 1.8 percent of the mass of water, and the hydrothermal reaction is carried out in a hydrothermal kettle with polytetrafluoroethylene as an inner container. The hydrothermal reaction was carried out under the conditions of heating at 210 ℃ for 25 hours and then cooling naturally after the reaction.
After full reaction, naturally cooling after the reaction is finished;
and (4) centrifugally separating and washing a product obtained by the reaction to obtain the molybdenum disulfide tin/tin disulfide nanosheet. The rotational speed of the centrifugal separation is 8000 r/min. The molybdenum disulfide tin/tin disulfide nanosheet is of a planar heterostructure.
And a surfactant is also added into the raw materials of the hydrothermal reaction, and the addition amount of the surfactant is 3% of the mass of water. The surfactant is polyvinylpyrrolidone. The molybdenum disulfide tin/tin disulfide nanosheet is of a core-shell structure.
Due to the excellent performances and diversity of the metal sulfide, the 2D planar heterojunction is a material with different components and does not have any covalent bond in the same planeAnd (4) sewing. Sn prepared by the invention0.5Mo0.5S2/SnS2The plane heterostructure breaks through the traditional gas phase preparation method of the plane heterostructure, and the plane heterostructure is prepared by a liquid phase method for the first time. The heterostructure has a unique heterogeneous interface with SnS2Compared with the nano sheet, the nano sheet has greatly improved conductivity, so that the nano sheet is suitable for the fields of sensors, photoelectric detection and the like.
Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can make modifications and equivalents to the specific embodiments of the present invention without departing from the spirit and scope of the present invention, which is set forth in the following claims.
Claims (6)
1. The preparation method of the molybdenum disulfide tin/tin disulfide nanosheet is characterized by comprising the following steps:
doping Sn with MoO3Nanoribbon, SnS2Mixing the nano-sheets with thiourea, and carrying out hydrothermal reaction by using water as a solvent;
naturally cooling after the full reaction is finished;
centrifugally separating and washing a product obtained by the reaction to obtain a molybdenum tin disulfide/tin disulfide nanosheet;
said Sn doped MoO3Nanoribbons and SnS2The mass ratio of the nano sheets is 1: (3-5), the addition amount of thiourea is 1% -2% of the mass of water, the hydrothermal reaction is carried out under the condition of heating at 200-220 ℃ for 20-40 hours, and the reaction is naturally cooled after the reaction is finished.
2. The method for preparing the molybdenum disulfide tin/tin disulfide nanosheet as claimed in claim 1, wherein the hydrothermal reaction is carried out in a hydrothermal kettle with polytetrafluoroethylene as an inner container.
3. The method for preparing the molybdenum disulfide tin/tin disulfide nanosheet as claimed in claim 1, wherein the rotational speed of the centrifugal separation is 8000 to 12000 r/min.
4. The method as claimed in any one of claims 1 to 3, wherein the Mo-Sn disulfide/Sn disulfide nanosheet is a planar heterostructure.
5. The method for preparing the molybdenum disulfide tin/tin disulfide nanosheet as claimed in claim 1, wherein a surfactant polyvinylpyrrolidone is further added to the raw materials of the hydrothermal reaction, wherein the amount of the surfactant added is 1% to 2% of the mass of the water.
6. The method for preparing the molybdenum disulfide tin/tin disulfide nanosheet as claimed in claim 5, wherein the molybdenum disulfide tin/tin disulfide nanosheet is of a core-shell structure.
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