CN114815502B - A method for preparing two-dimensional layered bismuth selenide nanosheets based on nanoimprinting - Google Patents
A method for preparing two-dimensional layered bismuth selenide nanosheets based on nanoimprinting Download PDFInfo
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Abstract
本发明公开了一种基于纳米压印的二维层状硒化铋纳米片制备方法，采用聚二甲基硅氧烷将硒化铋片附着于衬底上，然后将其整体放置于纳米压印机的工作台上，在不高于80℃以及在20～30bar压力下进行压印，得到硒化铋纳米片。本发明通过纳米压印对层间结合力强的硒化铋材料进行剥离制备，采用与硒化铋材料结合力好的衬底，在聚二甲基硅氧烷热释放温度以下以及稳定的压力氛围中，促使硒化铋厚片层与层之间的分离，从而获得厚度为十几纳米的硒化铋片。
The present invention discloses a method for preparing a two-dimensional layered bismuth selenide nanosheet based on nanoimprinting, wherein the bismuth selenide sheet is attached to a substrate using polydimethylsiloxane, and then the whole is placed on a workbench of a nanoimprinter, and imprinted at a temperature not higher than 80°C and a pressure of 20 to 30 bar to obtain a bismuth selenide nanosheet. The present invention peels off a bismuth selenide material with strong interlayer bonding strength through nanoimprinting, and uses a substrate with good bonding strength with the bismuth selenide material to promote the separation of thick bismuth selenide sheets below the thermal release temperature of polydimethylsiloxane and in a stable pressure atmosphere, thereby obtaining a bismuth selenide sheet with a thickness of more than ten nanometers.
Description
Technical Field
The invention relates to a preparation method of a two-dimensional layered bismuth selenide nano-sheet based on nano-imprinting.
Background
Since graphene was first discovered in 2004, there has been an increasing search for two-dimensional materials. The continuous improvement of the two-dimensional material preparation technology and the treatment of atomic-scale materials greatly promote the development of two-dimensional materials and two-dimensional equipment. Two-dimensional materials are also widely used in electronics, optoelectronics, topospin electronics, biological application energy storage and energy conversion devices, and other fields. The tape mechanical stripping is a common preparation method of two-dimensional materials, but the method has the problems of low yield, small transverse dimension of samples obtained by stripping and the like, and the efficiency of preparing the two-dimensional layered bismuth selenide by adopting the tape mechanical stripping method is further reduced and the two-dimensional layered bismuth selenide with the thickness of tens of nanometers cannot be obtained in the face of layered materials with stronger binding energy such as bismuth selenide. The nano imprinting is used as a micro-nano processing method, is one of the alternative means of photoetching, can prepare an array structure in a large scale, and has the advantages of low cost, high flux, high resolution and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a two-dimensional layered bismuth selenide nano sheet based on nano imprinting, which can obviously improve the preparation efficiency of the bismuth selenide nano sheet, namely, a plurality of samples can be prepared on a sample table at the same time, and the bismuth selenide nano sheet with the thickness of tens of nanometers can be obtained on a substrate.
According to the technical scheme, the preparation method of the two-dimensional layered bismuth selenide nano-sheet based on nano-imprinting comprises the steps of adhering the bismuth selenide sheet to a substrate by adopting polydimethylsiloxane, and then placing the whole bismuth selenide sheet on a workbench of a nano-imprinting machine for imprinting at a temperature of not higher than 80 ℃ and a pressure of 20-30 bar to obtain the bismuth selenide nano-sheet.
The process of adhering bismuth selenide piece to substrate by adopting polydimethylsiloxane comprises the steps of adhering bismuth selenide block by using adhesive tape to obtain adhesive tape with bismuth selenide thick piece, adhering one surface of the adhesive tape with bismuth selenide thick piece to polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering, transferring part of bismuth selenide thick piece on the adhesive tape to polydimethylsiloxane to obtain polydimethylsiloxane adhered with bismuth selenide piece, and adhering one surface of the polydimethylsiloxane adhered with bismuth selenide piece to substrate to enable bismuth selenide piece to be adhered to substrate.
Wherein the thickness of the bismuth selenide sheet on the polydimethylsiloxane is 10-60 mu m.
Wherein the bonding time of the adhesive tape and the polydimethylsiloxane is 2-10 minutes.
The substrate is a silicon wafer substrate with a silicon oxide layer or an aluminum oxide layer, the thickness of the silicon oxide layer is 300nm, and the aluminum oxide layer is obtained by depositing an atomic layer deposition system on the surface of the silicon wafer, wherein the thickness of the silicon wafer is 30nm.
The thickness of the bismuth selenide nano-sheet is 10-19 nm.
Wherein the imprinting time is 60 s-120 s.
The silicon wafer substrate with the silicon oxide layer or the aluminum oxide layer has high bonding energy with bismuth selenide material (the bonding energy obtained by subtracting the surface energy of the silicon wafer substrate and the bismuth selenide material from the attached energy is higher, the bismuth selenide thin sheet with low nanometer thickness is easier to generate), the nano imprinting provides stable temperature and pressure, and the peeling of the two-dimensional layered bismuth selenide is realized under the condition that the heat release temperature (80 ℃) of polydimethylsiloxane is lower (when the temperature is higher than 80 ℃), the adhesion between the polydimethylsiloxane and the bismuth selenide is not favorable for peeling the bismuth selenide nano sheet, and when the temperature is 50-70 ℃), the adhesion between the polydimethylsiloxane and the bismuth selenide is weakened.
The method has the beneficial effects that the bismuth selenide material with strong interlayer binding force is stripped and prepared by nano imprinting, and the bismuth selenide sheet with the thickness of tens of nanometers is obtained by adopting the substrate with good binding force with the bismuth selenide material and promoting the separation between bismuth selenide thick sheet layers in a stable pressure atmosphere under the heat release temperature of polydimethylsiloxane.
Drawings
FIG. 1 is a flow chart of a method for preparing bismuth selenide nanosheets of the present invention;
FIG. 2 is a Raman spectrum of the bismuth selenide nanosheets prepared in example 1;
FIG. 3 is an atomic force microscope image and thickness of bismuth selenide nanoplatelets prepared in example 1;
FIG. 4 is a Raman spectrum of the bismuth selenide nanosheets prepared in example 2;
FIG. 5 is an atomic force microscope image and thickness of bismuth selenide nanoplatelets prepared in example 2;
FIG. 6 is a Raman spectrum of the bismuth selenide nanosheets prepared in example 3;
FIG. 7 is an atomic force microscope image and thickness of bismuth selenide nanoplatelets prepared in example 3;
FIG. 8 is a Raman spectrum of the bismuth selenide nanosheets prepared in example 4;
fig. 9 is an atomic force microscope image and thickness of the bismuth selenide nanosheets prepared in example 4.
Detailed Description
Example 1
As shown in fig. 1, the preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 2 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to be 50 ℃, the pressure is 20bar, and the imprinting time is 60s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
The obtained bismuth selenide nano-sheet is subjected to spectrum characterization by using a confocal Raman microscope, the test result is shown in figure 2, the phase characterization result shows that the Raman peak of the nano-sheet has no obvious difference with the Raman peak position of a bismuth selenide block, the appearance and the thickness of the bismuth selenide nano-sheet are characterized by using an atomic force microscope, the surface of the layered material is flat, the thickness is 19.10nm, and the test result is shown in figure 3.
Example 2
The preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 10 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to 70 ℃, the pressure is 20bar, and the imprinting time is 120s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
The obtained bismuth selenide nano-sheet is subjected to spectrum characterization by using a confocal Raman microscope, the test result is shown in figure 4, the phase characterization result shows that the Raman peak of the nano-sheet has no obvious difference with the Raman peak position of a bismuth selenide block, the appearance and the thickness of the bismuth selenide nano-sheet are characterized by using an atomic force microscope, the surface of the layered material is flat, the thickness is 9.98nm, and the test result is shown in figure 5.
Example 3
The preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 2 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to be 50 ℃, the pressure is 20bar, and the imprinting time is 60s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
The obtained bismuth selenide nano-sheet is subjected to spectrum characterization by using a confocal Raman microscope, the test result is shown in figure 6, the phase characterization result shows that the Raman peak of the nano-sheet has no obvious difference with the Raman peak position of a bismuth selenide block, the appearance and the thickness of the bismuth selenide nano-sheet are characterized by using an atomic force microscope, the surface of the layered material is flat, the thickness is 17.67nm, and the test result is shown in figure 7.
Example 4
The preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 10 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to 70 ℃, the pressure is 20bar, and the imprinting time is 120s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
The obtained bismuth selenide nano-sheet is subjected to spectrum characterization by using a confocal Raman microscope, the test result is shown in figure 8, the phase characterization result shows that the Raman peak of the nano-sheet has no obvious difference with the Raman peak position of a bismuth selenide block, the appearance and the thickness of the bismuth selenide nano-sheet are characterized by using an atomic force microscope, the surface of the layered material is flat, the thickness is 14.38nm, and the test result is shown in figure 9.
Examples 1 to 4 illustrate that bismuth selenide nanoplatelets having a thickness of tens of nanometers can be obtained by controlling the imprinting temperature at 50 ℃ to 70 ℃ and the pressure at 20 bar. The temperature rise causes a further reduction in the thickness of the flakes for the same substrate, the resulting nanoplatelets on the respective substrate being thinner at a temperature of 70 ℃ and a pressure of 20bar, this trend of variation being more pronounced on a silicon oxide substrate than on an aluminum oxide substrate, the effect of the temperature change on the thickness of the flakes for the different substrates not being a temperature rise, the relationship of the thinner flakes, this being related to the characteristics of the substrate itself.
Comparative example 1
The preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 10 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to 90 ℃, the pressure is 20bar, and the imprinting time is 120s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
And (3) carrying out morphology and thickness characterization on the bismuth selenide nano-sheet by using an atomic force microscope, wherein the surface of the layered material is smooth, and the thickness is 83.55nm.
Comparative example 2
The preparation method of the bismuth selenide nano-sheet comprises the following steps:
(1) The method comprises the steps of adhering bismuth selenide blocks by using an adhesive tape, separating to obtain an adhesive tape with bismuth selenide thick sheets, adhering one surface of the adhesive tape with the bismuth selenide thick sheets to the polydimethylsiloxane, separating the adhesive tape and the polydimethylsiloxane after adhering for 10 minutes, and transferring the bismuth selenide thick sheets on the adhesive tape to the polydimethylsiloxane to obtain the polydimethylsiloxane adhered with the bismuth selenide sheets;
(2) The imprinting temperature is adjusted to 70 ℃, the pressure is 30bar, and the imprinting time is 120s;
(3) And after the experiment is finished and the temperature is reduced to the room temperature, the silicon wafer substrate with the layered bismuth selenide nano-sheets is obtained.
And (3) carrying out morphology and thickness characterization on the bismuth selenide nano-sheet by using an atomic force microscope, wherein the surface of the layered material is smooth, and the thickness is 37.93nm.
Comparative examples 1-2 demonstrate that when the temperature exceeds 70 ℃ or the imprint pressure is higher than 20bar, the bonding force of the bismuth selenide thick sheet and the polydimethylsiloxane is weakened, resulting in a rapid increase in the thickness of the nano sheet on the substrate.
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| CN103641079A (en) * | 2013-10-21 | 2014-03-19 | 东南大学 | Preparation method for large-size ultrathin bismuth selenide nanosheet |
| CN105301909A (en) * | 2015-09-22 | 2016-02-03 | 北京大学 | Method for preparing micro-belt or nano-belt of two-dimensional nanomaterial |
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| US7252862B2 (en) * | 2004-08-30 | 2007-08-07 | Hewlett-Packard Development Company, L.P. | Increasing adhesion in an imprinting procedure |
| JP2012183753A (en) * | 2011-03-07 | 2012-09-27 | Fujifilm Corp | Nanoimprinting method |
| KR101436911B1 (en) * | 2012-04-25 | 2014-09-02 | 그래핀스퀘어 주식회사 | Patterning method of graphene using hot embossing imprinting |
| KR102513763B1 (en) * | 2014-06-20 | 2023-03-24 | 더 리전트 오브 더 유니버시티 오브 캘리포니아 | Method for the fabrication and transfer of graphene |
| CN111229199A (en) * | 2019-10-09 | 2020-06-05 | 武汉纺织大学 | Method and application of two-dimensional bismuth-based oxo compound nanosheets prepared by liquid phase exfoliation |
| CN114197051B (en) * | 2021-12-08 | 2024-03-15 | 电子科技大学长三角研究院(湖州) | Self-supporting two-dimensional selenium oxide nanosheet array and preparation method thereof |
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| CN103641079A (en) * | 2013-10-21 | 2014-03-19 | 东南大学 | Preparation method for large-size ultrathin bismuth selenide nanosheet |
| CN105301909A (en) * | 2015-09-22 | 2016-02-03 | 北京大学 | Method for preparing micro-belt or nano-belt of two-dimensional nanomaterial |
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