CN116984623B - Two-dimensional bismuth nanocrystal synthesis method based on sectional hydrothermal method - Google Patents
Two-dimensional bismuth nanocrystal synthesis method based on sectional hydrothermal method Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 88
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 47
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 39
- 238000001308 synthesis method Methods 0.000 title claims abstract description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 90
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 72
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 72
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 72
- QKDFWYFCMLUTQD-UHFFFAOYSA-N 17-bromo-N,N-dimethylheptadecan-1-amine Chemical compound BrCCCCCCCCCCCCCCCCCN(C)C QKDFWYFCMLUTQD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 14
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 14
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- 239000000047 product Substances 0.000 description 60
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 31
- 229910052710 silicon Inorganic materials 0.000 description 31
- 239000010703 silicon Substances 0.000 description 31
- 239000013078 crystal Substances 0.000 description 22
- 239000002135 nanosheet Substances 0.000 description 22
- 239000012535 impurity Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- 238000001069 Raman spectroscopy Methods 0.000 description 12
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 239000005922 Phosphane Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
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- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
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- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
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- -1 silylene, germylene Chemical group 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
Abstract
The invention discloses a two-dimensional bismuth nanocrystal synthesis method based on a sectional hydrothermal method, which comprises the following steps: uniformly dispersing sodium bismuthate into glycerol solution to obtain a first solution with the concentration of 0.025-0.075 mol/L; fully dissolving bromohexadecyl trimethylamine and polyvinylpyrrolidone in a molar ratio of 1:0.5-1:3.5 in a glycerol solution to form a second solution; fully mixing the first solution and the second solution with equal volumes to obtain a third solution; a first hydrothermal stage: heating the third solution to 30-80 ℃, and preserving heat for at least 5 hours; a second hydrothermal stage: and heating the third solution to 160-200 ℃ and preserving heat for more than 20 hours, and cooling and centrifugally separating to obtain the two-dimensional bismuth nanocrystals.
Description
Technical Field
The invention belongs to the technical field of low-dimensional nanomaterial preparation, and particularly relates to a two-dimensional bismuth nano-synthesis method based on a sectional hydrothermal method.
Background
Following the development of the black phosphane, monoatomic layer two-dimensional materials of other elements of the fifth main group (As, sb, bi) were also developed successively. Among them, two-dimensional bismuth (bisnuthene) attracts a lot of attention due to its unique topological insulator properties and giant magnetoresistance effect, and there are predictions that bismuth, after being reduced in dimension, will exhibit properties different from its bulk material, such as semiconductor characteristics. In addition, the two-dimensional bismuth electrocatalyst can play an important role in enhancing the cycle life and improving the electrochemical activity at certain sites in the field of high-performance sodium ion batteries. Two-dimensional bismuth is calculated to be superior to silylene, germylene, phosphazene and arsene in air stability, which makes it of great potential in high performance electronics and communications. Bismuth, on the other hand, has a specific metallic surface state on the surface and a very high carrier concentration. Due to the very strong spin-orbit coupling, its surface has spin-cleavage properties, which make two-dimensional bismuth a potential information material for the development of new generation spintronics devices.
Many attempts are currently made at the synthesis of two-dimensional bismuth nanoplatelets at home and abroad. Among these, the most common is the vapor deposition approach, since the atomic structure of bismuth is not lamellar in itself, and most importantly, the melting point of the material is low. Moreover, the method has a plurality of defects such as lower yield, slower reaction speed and poor repeatability. The synthesis of bismuth nanowires is reported by vapor deposition reported at present, but bismuth two-dimensional morphology with large grain size and atomic-scale thickness is not synthesized yet. Atomic epitaxy is also used to synthesize two-dimensional bismuth, but it is reported in literature that the two-dimensional bismuth synthesized by this method is only a few hundred nanometers wide in the lateral direction, and that this method relies on the selection of a substrate material with a suitable crystal orientation, which presents a high challenge for the next device fabrication and processing. Meanwhile, the bismuth nanosheets are prepared by a liquid phase intercalation method in the prior art, and the method can obtain nano products with larger yield, but has poor controllability, and particles of the products are only hundreds of nanometers in size, so that the bismuth nanosheets are not suitable for later-stage spintronic devices and are used for battery energy storage.
The hydrothermal synthesis method has the characteristics of large and controllable product quantity and low temperature, so the hydrothermal synthesis method is used for trying the synthesis of the two-dimensional nanomaterial. In early researches, researchers successfully synthesize bismuth nanospheres and nanowires by a hydrothermal method, and the yield is high. However, the hydrothermal method is not used for successfully synthesizing the nano-sheets with the micro-scale size and the atomic-scale thickness, which is because the reaction is fast, and the nano-sheets can spontaneously react at room temperature, so that the use requirement on the coating agent is very high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a two-dimensional bismuth nano-synthesis method based on a sectional hydrothermal method.
According to a first aspect of an embodiment of the present invention, there is provided a two-dimensional bismuth nanocrystal synthesis method based on a segmented hydrothermal method, the method comprising:
uniformly dispersing sodium bismuthate into glycerol solution to obtain a first solution with the concentration of 0.0025-0.075 mol/L;
fully dissolving bromohexadecyl trimethylamine and polyvinylpyrrolidone in a molar ratio of 1:0.5-1:3.5 in a glycerol solution to form a second solution;
fully mixing the first solution and the second solution with equal volumes to obtain a third solution;
a first hydrothermal stage: heating the third solution to 30-80 ℃, and preserving heat for at least 5 hours;
a second hydrothermal stage: and heating the third solution to 160-200 ℃ and preserving heat for more than 20 hours, and cooling and centrifugally separating to obtain the two-dimensional bismuth nanocrystals.
Further, the concentration of the first solution was 0.05 mol/L.
Further, the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:2.5.
Further, in the first hydrothermal stage, the third solution was heated to 50 ℃ and incubated for 8 hours.
Further, in the second hydrothermal stage, the third solution is heated to 180 ℃.
According to a second aspect of the embodiment of the invention, a two-dimensional bismuth nanocrystal is provided, which is prepared by the two-dimensional bismuth nanocrystal synthesis method based on the segmented hydrothermal method.
According to a third aspect of embodiments of the present invention, there is provided an electronic device, including an electronic device body and the above two-dimensional bismuth nanocrystals disposed on the electronic device body.
According to a fourth aspect of embodiments of the present invention there is provided the use of two-dimensional bismuth nanocrystals in low temperature superconductivity.
According to a fifth aspect of embodiments of the present invention, there is provided the use of two-dimensional bismuth nanocrystals in photothermal conversion medium materials.
According to a sixth aspect of the embodiment of the invention, there is provided an application of a two-dimensional bismuth nanocrystal in mid-far infrared light detection of photosensitive materials.
The beneficial effects of the invention are as follows:
(1) The present invention prepares the first solution from glycerol, which itself is a solution environment that provides the reaction and is also a reducing agent for the reaction process.
(2) The invention prepares the two-dimensional bismuth nanosheets with high quality, atomic-scale thickness, micron-scale width and high yield based on the sectional hydrothermal method. The first hydrothermal stage utilizes the steric hindrance effect of two cladding agents of bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) on different crystal faces to realize crystal orientation control and limit growth in a seed crystal nucleation stage; the second hydrothermal stage continues to provide a high pressure hydrothermal environment that continues to grow in the width direction. Finally, the synthesis of the high-yield two-dimensional bismuth nanosheets is realized. The present invention utilizes a segmented approach to maximize the action of the surfactant while controlling the rate of nucleation and growth.
(3) The two-dimensional bismuth nano-sheet prepared by the invention shows the phenomenon of Raman shift with different thicknesses. Meanwhile, the high conductivity and the thickness-related conductivity of the micro-nano-processed two-end device can be obtained through testing. The two-dimensional bismuth nanoplatelets of this size provide a material basis for its future device fabrication and testing.
(4) The preparation method has the advantages of simple and controllable process, short preparation period, safety, no pollution and low cost. According to the actual production requirement, the two-dimensional bismuth nanosheets can be flexibly prepared, so that the method becomes an effective technical means for developing a new generation of spin electronic devices.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
Fig. 1 is a schematic flow chart of a two-dimensional bismuth nanocrystal synthesis method based on a segmented hydrothermal method according to an embodiment of the present invention;
FIG. 2 is a photograph of a high power microscope of a two-dimensional bismuth nanoplatelet prepared according to the preferred embodiment of example 1 of the present invention;
FIG. 3 is a graph showing the results of an Atomic Force Scanning Electron Microscope (AFSEM) of a two-dimensional bismuth nanosheet prepared according to a preferred embodiment of the present invention in example 1;
FIG. 4 is a graph showing the result of X-ray diffraction spectrum of the two-dimensional bismuth nanoplatelets prepared according to the preferred embodiment of example 1 of the present invention;
FIG. 5 is a schematic diagram of the transmission electron microscope characterization result and the related atomic structure of the two-dimensional bismuth nanoplatelets prepared according to the preferred embodiment of example 1 of the present invention;
fig. 6 is a graph showing raman scattering results of the two-dimensional bismuth nanoplatelets prepared according to the preferred embodiment of the present invention in terms of thickness;
fig. 7 is a schematic representation of the electronic device and basic electrical characterization of a two-dimensional bismuth nanoplatelet prepared according to the preferred embodiment of example 1 of the present invention;
FIG. 8 is a photomicrograph of the reaction product of example 2 of the present invention;
FIG. 9 is a photomicrograph of the reaction product of example 3 of the present invention;
FIG. 10 is a photomicrograph of the reaction product of example 4 of the present invention;
FIG. 11 is a photomicrograph of the reaction product of example 5 of the present invention;
FIG. 12 is a photomicrograph of the reaction product of example 6 of the present invention;
FIG. 13 is a photomicrograph of the reaction product of example 7 of the present invention;
FIG. 14 is a photomicrograph of the reaction product of example 8 of the present invention;
FIG. 15 is a photomicrograph of the reaction product of example 9 of the present invention;
FIG. 16 is a photomicrograph of the reaction product of example 10 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The features of the following examples and embodiments may be combined with each other without any conflict.
The embodiment of the invention provides a two-dimensional bismuth nano crystal synthesis method based on a sectional hydrothermal method, which is used for synthesizing two-dimensional bismuth nano sheets with atomic-scale thickness and micron-scale width. The invention designs two stages to accurately control the nucleation and growth of bismuth nanoplatelets. The dimensional control of the seed crystal is realized by utilizing the restriction of two different coating agents of bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) on the growth of different crystal faces under the condition of lower temperature. And providing a high-temperature and high-pressure environment in the next step to grow the large-scale two-dimensional bismuth nano-sheet. Meanwhile, the invention performs certain optical characterization on the synthesized bismuth, discovers the law of Raman scattering along with thickness variation, and detects the good conductivity by manufacturing devices at two ends.
As shown in fig. 1, the two-dimensional bismuth nanocrystal synthesis method based on the segmented hydrothermal method provided by the invention specifically comprises the following steps:
uniformly dispersing sodium bismuthate into glycerol solution to obtain a first solution with the concentration of 0.0025-0.075 mol/L; preferably, the concentration of the first solution is 0.05 mol/L.
The glycerol solution itself provides the solution environment for the reaction and is also the reducing agent for the reaction process.
Fully dissolving bromohexadecyl trimethylamine and polyvinylpyrrolidone in a molar ratio of 1:0.5-1:3.5 in a glycerol solution to form a second solution; preferably, the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:2.5.
Fully mixing the first solution and the second solution with equal volumes to obtain a third solution;
a first hydrothermal stage: heating the third solution to 30-80 ℃, and preserving heat for at least 5 hours; preferably, in the first hydrothermal stage, the third solution is heated to 50 ℃ and incubated for 8 hours.
In the first hydrothermal stage, the steric hindrance effect of two cladding agents of bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) on different crystal faces is utilized to realize crystal orientation control, carry out crystal face cladding and limit the nucleation growth of the two-dimensional bismuth nano crystal seeds.
A second hydrothermal stage: and heating the third solution to 160-200 ℃ and preserving heat for more than 20 hours, and cooling and centrifugally separating to obtain the two-dimensional bismuth nanocrystals. Preferably, in the second hydrothermal stage, the third solution is heated to 180 ℃.
In the second hydrothermal stage, a high-pressure hydrothermal environment is provided to allow the two-dimensional bismuth nano-seed crystal to continue to grow in the width direction.
The two-dimensional bismuth nanocrystal synthesis method based on the segmented hydrothermal method provided by the invention is described below by combining with an embodiment.
Example 1
Embodiment 1 of the present invention is a preferred embodiment, and specifically includes:
step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution were thoroughly mixed by a stirrer to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 o And C, maintaining the temperature for 8 hours for standby. It was found that the third solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: then the third solution is put into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is heated to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer and the copper mesh with deionized water for three times, and then transferring the silicon wafer and the copper mesh to perform X-ray diffraction spectrum, scanning electron microscope and transmission electron microscope picture characterization on the silicon wafer and the copper mesh.
The photograph of the product obtained in the embodiment 1 of the invention under the high power microscope is shown in fig. 2, the thickness and the basic morphology of the product are represented under the atomic force scanning electron microscope, the X-ray diffraction spectrum of the product is shown in fig. 3, the transmission electron microscope and the high resolution transmission diagram are shown in fig. 4, and the three-dimensional atomic structure deduced from the high resolution diagram is shown in fig. 5.
As shown in FIGS. 2-5, the large-scale two-dimensional bismuth nanosheets prepared in the embodiment 1 of the invention have atomic-scale thickness, generate a two-dimensional triangle shape, have triangular side lengths of about 10 microns, have uniform shape, higher yield, larger grain size and fewer impurities.
Step S6: the clean product was transferred to a silicon wafer and its raman scattering optical characteristics were characterized using a raman test analyzer. And preparing metal electrodes at two ends by utilizing a micro-nano processing technology, and testing the electrical characteristics of the metal electrodes. The raman versus thickness characteristic is shown in fig. 6. The resulting device and basic electrical characteristics are shown in fig. 7, where (a) in fig. 7 is a voltage-current graph of the device prepared in example 1, (B) in fig. 7 is a voltage-resistance graph of the device prepared in example 1, and (C) in fig. 7 is an optical microscope image of the device prepared in example 1, and it is known from (C) in fig. 7 that the device has no open circuit or short circuit condition.
As can be seen from fig. 6, the two-dimensional bismuth nanoplatelets prepared in example 1 of the present invention exhibit raman shift phenomena with different thicknesses. In particular, when raman characterization is performed with two-dimensional bismuth nanoplatelets of different thickness, two atomic vibration modes (mode E g And mode A 1g ），E g Mode and A 1g The modes all have offset characteristics, wherein a change curve chart of the thickness of the two-dimensional bismuth nano sheet can be extracted from the Raman offset curve chart, and as the thickness is increased, the Raman offset value is gradually reduced, and E is known from FIG. 6 g Mode and A 1g The patterns all show the same trend of variation. Wherein E is g The mode represents a "symmetric stretching" (Symmetric Stretch) vibration mode which involves simultaneous outward or inward vibration of adjacent atoms (typically atoms of the same species) in the crystal to maintain symmetry of the crystal; in Raman spectroscopy, E g Vibration generally exhibits a peak of high intensity, corresponding to a strong interaction between atoms in the crystal structure. A is that 1g The mode represents an "asymmetric stretching" (Asymmetric Stretch) vibration mode which involves asymmetric vibration of atoms in the crystal, some of which vibrate outwards and others of which vibrate inwards.
Meanwhile, through testing of the two-end devices after micro-nano processing, the two-end devices prepared from the two-dimensional bismuth nanosheets prepared in the embodiment 1 have better conductivity and conductivity related to thickness. The two-dimensional bismuth nanoplatelets of this size provide a material basis for its future device fabrication and testing.
Example 2
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: and placing the third solution into a hydrothermal reaction kettle. Heating the hydrothermal reaction kettle to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 8.
The first hydrothermal stage of the staged hydrothermal process (i.e., no crystal face coating at the initial stage of nucleation) was removed in this example 2, and the coating agents bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) and other materials were directly carried out in a high temperature reactor in this example 2. The product obtained in example 2 was all bismuth nanowires, as shown in fig. 8, due to failure to achieve coating of the seed crystal on the appropriate crystal plane.
It is clear that the first hydrothermal stage in the staged hydrothermal process is an essential step for crystal face cladding in the initial nucleation stage by bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) as cladding agents.
Example 3
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:0.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S2: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 o And C, maintaining the temperature for 8 hours for standby. It was found that the third solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: placing the third solution into a hydrothermal reaction kettle, and heating the hydrothermal reaction kettle to 180 DEG Co C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 9.
In example 2 of the present invention, the molar ratio of bromohexadecyl trimethylamine (CTAB) to polyvinylpyrrolidone (PVP) was set to 1:0.5, so that the ratio of polyvinylpyrrolidone (PVP) was reduced. As shown in FIG. 9, the product obtained in example 2 had a two-dimensional morphology but had many impurities, and its morphology was not uniform. It can be seen that the ratio of the two coating agents cetyltrimethylamine bromide (CTAB) and polyvinylpyrrolidone (PVP) is very important.
Example 4
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:3.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 o And C, maintaining the temperature for 8 hours for standby. It was found that the third solution changed from pale yellow to pale white.
Step S5:placing the third solution into a hydrothermal reaction kettle, and heating the hydrothermal reaction kettle to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 10.
In example 4 of the present invention, the molar ratio of bromohexadecyl trimethylamine (CTAB) to polyvinylpyrrolidone (PVP) was set to 1:3.5, so that the duty ratio of polyvinylpyrrolidone (PVP) was increased, and as shown in fig. 10, the product obtained in example 4 had a two-dimensional morphology, and also had many impurities, and the morphology exhibited a hexagonal shape, but the grain size was smaller. It can be seen that the ratio of the two coating agents cetyltrimethylamine bromide (CTAB) and polyvinylpyrrolidone (PVP) is very important.
Example 5
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 30 o And C, maintaining the temperature for 8 hours for standby. It was found that the three solutions changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: placing the third solution into a hydrothermal reaction kettle, and heating the hydrothermal reaction kettle to 180 DEG Co C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 11.
Example 5 adjustment of the first hydrothermal stageIs set to 30 o C, as shown in FIG. 11, it was found that the product obtained in this example 5 was lower in yield and smaller in grain size despite the triangular morphology. Therefore, the holding temperature of the first hydrothermal stage is also a critical parameter.
Example 6
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 80 under the condition of the stirrer o And C, maintaining the temperature for 8 hours for standby. It was found that the third solution changed from pale yellow to pale white.
S5: a second hydrothermal stage: placing the third solution into a hydrothermal reaction kettle, and heating the hydrothermal reaction kettle to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 12.
In example 6, the holding temperature in the first hydrothermal stage was adjusted to 80 o C, as shown in FIG. 12, the product obtained in example 6 was lower in yield and smaller in grain size, although the triangular morphology was produced. Therefore, the heating temperature of the first step is also a critical parameter.
Example 7:
step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 under the condition of the stirrer o And C, maintaining the temperature for 5 hours for standby. It was found that the third solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: then the third solution is put into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is heated to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 13.
In this example 7, the heat-retaining period of the first hydrothermal stage was adjusted, the heating time was reduced, and the heating time was set to 5 hours, as shown in fig. 13, and the yield was low in the product obtained in this example 7 although the triangular morphology was generated. It follows that the length of the first hydrothermal stage is also a critical parameter for the preparation and can affect the full action of the coating agent.
Example 8
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 under the condition of the stirrer o And C, keeping the temperature for 10 hours for standby. The third solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: then the third solution is put into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is heated to 180 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The micrograph is shown in FIG. 14.
In this example 8, the heat-preserving period of the first hydrothermal stage was adjusted, and the heating time was set to 10 hours, and as is clear from fig. 14, the product obtained in this example 8 had a triangular morphology and a higher yield, but compared with the preferred embodiment example 1, the product had more impurities, and some nanowires and particles had more impurities. It follows that the length of the incubation period of the first hydrothermal stage is also a key parameter for the preparation.
Example 9
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 under the condition of the stirrer o And C, maintaining the temperature for 8 hours for standby. It was found that the third solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: then the third solution is put into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is heated to 160 DEG C o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The scanning electron microscope photograph is shown in FIG. 15.
In example 9, the holding temperature of the second hydrothermal stage was adjusted to 160 o As is clear from fig. 15, the product obtained in example 9 had a triangular morphology, but was more contaminated than in example 1, which is a preferred embodiment. It follows that the holding temperature of the second hydrothermal stage is also a key parameter for the preparation.
Example 10
Step S1: 0.35g of pale yellow sodium bismuth oxide was uniformly dispersed into the glycerol solution, stirred under a magnetic stirrer for a long period of time (24 hours), the solution was observed to become pale yellow, and upon standing for a period of time, no yellow precipitate was generated, forming a first solution having a concentration of 0.05 mol/L.
Step S2: bromohexadecyl trimethylamine (CTAB) and polyvinylpyrrolidone (PVP) were dissolved in a molar ratio of 1:2.5 to form a second solution in 30mL glycerol solution. Wherein the mass of polyvinylpyrrolidone (PVP) is 0.5g.
Step S3: equal volumes of the first solution and the second solution are thoroughly mixed to form a third solution.
Step S4: a first hydrothermal stage: placing the third solution in a stirrer, heating to 50 under the condition of the stirrer o And C, maintaining the temperature for 8 hours for standby. It was found that the solution changed from pale yellow to pale white.
Step S5: a second hydrothermal stage: then the third solution is put into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is heated to 200 o C was kept for 20 hours, and the product was obtained as a brown product by cooling and centrifuging. And (3) cleaning the silicon wafer with deionized water for three times, and transferring the silicon wafer to a silicon wafer respectively. The scanning electron microscope photograph is shown in FIG. 16.
In example 9, the holding temperature in the second hydrothermal stage was adjusted to 200 o C, as can be seen from FIG. 16, the present embodimentThe product of example 9 had a triangular morphology but was more contaminated than the preferred embodiment example 1. Therefore, the heat preservation temperature of the second hydrothermal stage is also a key parameter for preparation, and the impurities of the product are more under the condition that the heat preservation temperature of the second hydrothermal stage is higher.
Example 11
The only difference compared to example 1 is that the concentration of the first solution is 0.025 mol/L. A photomicrograph of the product of example 11 was taken, and the product of example 11 produced a two-dimensional triangular morphology with uniform morphology and less impurities.
Example 12
The difference compared to example 1 is only that the concentration of the first solution is 0.04 mol/L. A photomicrograph of the product of example 12 was taken, and the product of example 12 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 13
The difference compared to example 1 is only that the concentration of the first solution is 0.06 mol/L. A photomicrograph of the product of example 13 was taken, and the product of example 13 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 14
The only difference compared to example 1 is that the concentration of the first solution is 0.075mol/L. A photomicrograph of the product of example 14 was taken, and the product of example 14 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 15
The only difference compared to example 1 is that the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:1. A photomicrograph of the product of example 15 was taken, and the product of example 15 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 16
The only difference compared to example 1 is that the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:2. A photomicrograph of the product of example 16 was taken, and the product of example 16 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 17
The only difference compared to example 1 is that the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:3. A photomicrograph of the product of example 17 was taken, and the product of example 17 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 18
The only difference compared to example 1 is that in the first hydrothermal stage the third solution is heated to 40 ℃ and incubated for 6 hours. A photomicrograph of the product of example 18 was taken, and the product of example 18 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 19
The only difference compared to example 1 is that in the first hydrothermal stage the third solution is heated to 60 ℃ and incubated for 8 hours. A photomicrograph of the product of example 19 was taken, and the product of example 19 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 20
The only difference compared to example 1 is that in the second hydrothermal stage the third solution is heated to 170 ℃ and incubated for 25 hours. A photomicrograph of the product of example 20 was taken, and the product of example 20 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
Example 21
The only difference compared to example 1 is that in the second hydrothermal stage the third solution is heated to 190 ℃ and incubated for 22 hours. A photomicrograph of the product of example 21 was taken, and the product of example 21 produced a two-dimensional triangular morphology, uniform morphology, and less impurities.
The embodiment of the invention also provides a two-dimensional bismuth nanocrystal which is prepared by the two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method.
The embodiment of the invention also provides an electronic device, which comprises an electronic device main body and the two-dimensional bismuth nanocrystals, wherein the two-dimensional bismuth nanocrystals are arranged on the electronic device main body.
The embodiment of the invention also provides application of the two-dimensional bismuth nanocrystals in low-temperature superconductivity.
The embodiment of the invention also provides application of the two-dimensional bismuth nanocrystals in a photothermal conversion medium material.
The embodiment of the invention also provides application of the two-dimensional bismuth nanocrystals in mid-far infrared light detection photosensitive materials because the band gaps of the two-dimensional bismuth nanocrystals are smaller.
In summary, the two-dimensional bismuth nano-crystal synthesis method based on the sectional hydrothermal method provided by the invention has the advantages that the two-dimensional bismuth nano-sheet synthesized by the method has atomic-scale thickness, is triangular in shape, and has a side length of about 10 microns. In the method, the reduction speed of bismuth salt is very high, the seed crystal is required to be moderately controlled, the surfactant is effectively coated on a proper crystal face at a lower temperature, the seed crystal is completely coated, and the second step is added into a high-temperature hydrothermal reaction kettle for growth. The byproducts such as nanospheres, nanowires and the like are very easy to generate in the process of synthesizing the two-dimensional bismuth nanosheets, and important parameters such as the melting of a pre-coating agent and the time are required to be accurately controlled in the experimental process. Finally, the invention synthesizes the two-dimensional nano bismuth sheet with higher yield by a multi-stage reaction method, and characterizes the morphology and the crystal structure by SEM and AFM. Because the invention can synthesize nano sheets with a plurality of nano thickness, the Raman scattering spectrum is utilized to characterize the two-dimensional bismuth nano sheets with different thicknesses in the example, and the vibration mode of the two-dimensional bismuth nano sheets is found to deviate to a certain extent when the thickness is changed, so that the change of the optical property of the two-dimensional bismuth nano sheets under the thickness is revealed, and the efficiency is improved for preliminary judgment of the thickness of the two-dimensional bismuth nano sheets in the future. The two-dimensional bismuth nanosheets synthesized by the method have high yield and are easy to transfer to different substrates, and a material basis is provided for the application of the two-dimensional bismuth in the aspect of electronic and quantum devices in the future.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains. The specification and examples are to be regarded in an illustrative manner only.
It is to be understood that the present application is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof.
Claims (10)
1. A two-dimensional bismuth nanocrystal synthesis method based on a segmented hydrothermal method, which is characterized by comprising the following steps:
uniformly dispersing sodium bismuthate into glycerol solution to obtain a first solution with the concentration of 0.025-0.075 mol/L;
fully dissolving bromohexadecyl trimethylamine and polyvinylpyrrolidone in a molar ratio of 1:0.5-1:3.5 in a glycerol solution to form a second solution;
fully mixing the first solution and the second solution with equal volumes to obtain a third solution;
a first hydrothermal stage: heating the third solution to 30-80 ℃, and preserving heat for at least 5 hours;
a second hydrothermal stage: and heating the third solution to 160-200 ℃ and preserving heat for more than 20 hours, and cooling and centrifugally separating to obtain the two-dimensional bismuth nanocrystals.
2. The two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method according to claim 1, wherein the concentration of the first solution is 0.05 mol/L.
3. The two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method according to claim 1, wherein the molar ratio of bromohexadecyl trimethylamine to polyvinylpyrrolidone is 1:2.5.
4. The two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method according to claim 1, wherein in the first hydrothermal stage, the third solution is heated to 50 ℃ and kept for 8 hours.
5. The two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method according to claim 1, wherein in the second hydrothermal stage, the third solution is heated to 180 ℃.
6. A two-dimensional bismuth nanocrystal prepared by the two-dimensional bismuth nanocrystal synthesis method based on the sectional hydrothermal method according to any one of claims 1 to 5.
7. An electronic device comprising an electronic device body and the two-dimensional bismuth nanocrystal of claim 6 disposed on the electronic device body.
8. Use of the two-dimensional bismuth nanocrystals according to claim 6 in low temperature superconductivity.
9. Use of the two-dimensional bismuth nanocrystals according to claim 6 in photothermal conversion medium materials.
10. Use of the two-dimensional bismuth nanocrystals according to claim 6 for mid-far infrared light detection of photosensitive materials.
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