CN114772547A - Method for eliminating two-dimensional material wrinkles and application thereof - Google Patents

Method for eliminating two-dimensional material wrinkles and application thereof Download PDF

Info

Publication number
CN114772547A
CN114772547A CN202210374537.9A CN202210374537A CN114772547A CN 114772547 A CN114772547 A CN 114772547A CN 202210374537 A CN202210374537 A CN 202210374537A CN 114772547 A CN114772547 A CN 114772547A
Authority
CN
China
Prior art keywords
dimensional material
molybdenum disulfide
wrinkles
substrate
target substrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210374537.9A
Other languages
Chinese (zh)
Inventor
王嘉融
张光杰
裘晓辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Center for Nanosccience and Technology China
Original Assignee
National Center for Nanosccience and Technology China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by National Center for Nanosccience and Technology China filed Critical National Center for Nanosccience and Technology China
Priority to CN202210374537.9A priority Critical patent/CN114772547A/en
Publication of CN114772547A publication Critical patent/CN114772547A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/008Processes for improving the physical properties of a device
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B1/005Constitution or structural means for improving the physical properties of a device
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention provides a method for eliminating two-dimensional material wrinkles and application thereof. The method for eliminating the wrinkles of the two-dimensional material not only has the advantages of simple operation and high efficiency, but also has the advantage of little influence on the self properties of the two-dimensional material; meanwhile, the method provided by the invention can realize the elimination of the wrinkles of the two-dimensional material without special equipment and instruments in the operation process, has high elimination success rate, and provides a new thought for realizing the nondestructive transfer of the two-dimensional material.

Description

Method for eliminating two-dimensional material wrinkles and application thereof
Technical Field
The invention belongs to the technical field of two-dimensional materials, and particularly relates to a method for eliminating wrinkles of a two-dimensional material and application thereof.
Background
In recent years, two-dimensional transition metal chalcogenides such as molybdenum disulfide, tungsten diselenide and the like have excellent physical properties, and thus have great application potential in applications of optoelectronics, microelectronics and the like. In order to fabricate large-area devices, two-dimensional transition metal chalcogenides are often fabricated by chemical vapor deposition, however, substrates of integrated devices may not be resistant to corrosive and high temperature environments during chemical vapor growth, and thus, it is necessary to transfer a two-dimensional material from a growth substrate to a target substrate, and during the transfer, wrinkles and cracks are quite common, while the two-dimensional transition metal chalcogenides with wrinkles or cracks may also cause carrier scattering or short circuits, causing great damage to device integration, and thus, efforts are often made to develop lossless two-dimensional material transfer techniques.
At present, two-dimensional material transfer methods developed by people mainly comprise dry transfer and wet transfer, but the transfer technology without folds is often complex to operate and has low success rate. For the transferred sample, most of the sample is always wrinkled, so that the wrinkle removing technology is necessary to be developed. CN113264522A discloses a method for transferring two-dimensional materials, which comprises: the method comprises the steps of bonding one surface, provided with a two-dimensional material, of a growth substrate with a support layer through an adhesive layer, keeping the adhesive layer to have fluidity, removing the growth substrate from an etching solution, wherein the etching solution contains a low-boiling-point solvent with a boiling point lower than the curing temperature of the adhesive layer, heating at the temperature lower than the curing temperature of the adhesive layer, converting the low-boiling-point solvent into a gas state to prop open and eliminate wrinkles of the two-dimensional material, combining one surface, deviating from the support layer, of the two-dimensional material with a target substrate, removing the support layer and the adhesive layer, and transferring the two-dimensional material from the growth substrate to the target substrate. CN111285336A discloses a method for removing wrinkles from a two-dimensional material, the method comprising: providing a structure comprising a substrate and a two-dimensional material layer on a surface of the substrate; the structure has a first portion, a second portion, and an intermediate portion between the first and second portions, at least a portion of which is covered with the two-dimensional material; clamping the structure by clamping the first and second portions; and (b) subjecting the structure to tensile deformation, wherein the force causing the structure to tensile deformation is perpendicular to the two-dimensional material layer or parallel to the two-dimensional material layer at least at the initial stage, and the parallel to the two-dimensional material layer comprises superposition of the two-dimensional material layer. Including a process of subjecting a substrate having a two-dimensional material to tensile deformation. Controlled deformation of the substrate can be achieved by means of a punching or stretching device, whereby wrinkles in the two-dimensional material can be eliminated very well.
At present, in the prior art, annealing operation is often used to eliminate wrinkles of a two-dimensional material, but the method is not only low in efficiency, but also low in success rate, and the application of the two-dimensional material in device integration is limited.
Therefore, it is an urgent technical problem in the art to develop a method for removing wrinkles from a two-dimensional material with high efficiency, simple operation and high success rate.
Disclosure of Invention
In view of the shortcomings of the prior art, the present invention aims to provide a method for eliminating wrinkles of a two-dimensional material and an application thereof, wherein the method comprises the following steps: immersing the two-dimensional material attached to the target substrate into an intercalation agent, and performing annealing treatment to finish the elimination of folds of the two-dimensional material; the method is beneficial to eliminating wrinkles formed in the transfer process of the two-dimensional material, is simple to operate, has high success rate, realizes the lossless transfer of the two-dimensional material, and provides a new research idea for the two-dimensional material in the device integration application.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method of de-wrinkling a two-dimensional material, the method comprising: and (3) immersing the two-dimensional material attached to the target substrate into an intercalation agent, and performing annealing treatment to finish the elimination of the wrinkles of the two-dimensional material.
In the method provided by the invention, the wrinkles of the two-dimensional material are generated in the transfer process of the two-dimensional material, and further, the wrinkles are generated due to local deformation of the two-dimensional material caused by nonuniform stress distribution when the two-dimensional material is attached to a target substrate. Specifically, the method provided by the invention is mainly characterized in that an intercalator is inserted between the interfaces of the two-dimensional material and the target substrate to decouple the two-dimensional material and the target substrate, the stress on the two-dimensional material in the transfer process is released, the intercalator is removed by annealing treatment, the two-dimensional material without folds can be obtained, and the folds of the two-dimensional material are eliminated.
The method for eliminating the two-dimensional material wrinkles, provided by the invention, has the advantages of simplicity in operation, high efficiency and small influence on the properties of the material, can realize the elimination of the two-dimensional material wrinkles without special equipment and instruments in the operation process, has high success rate, and provides a new idea for realizing the nondestructive transfer of the two-dimensional material.
It should be noted that, in the method provided by the present invention, the atomic force microscope is used to observe the two-dimensional material attached to the target substrate before and after the intercalation agent is immersed, and if the two-dimensional material is observed to have wrinkles after the intercalation agent is immersed, the immersion step can be repeated until no wrinkles are observed, and then the annealing step is performed.
Preferably, the two-dimensional material comprises any one of graphene, graphene oxide, hexagonal boron nitride or a transition metal chalcogenide.
Preferably, the transition metal chalcogenide compound includes any one of molybdenum disulfide, molybdenum diselenide, or tungsten diselenide.
Preferably, the thickness of the two-dimensional material in step (1) is 0.3-30 nm, such as 0.5nm, 0.8nm, 1nm, 4nm, 8nm, 12nm, 16nm, 20nm, 24nm or 28 nm.
Preferably, the target substrate comprises a silicon substrate or a silicon nitride substrate.
Preferably, the two-dimensional material attached to the target substrate is prepared by a method comprising: and transferring the two-dimensional material mechanically stripped on the growth substrate to a target substrate to obtain the two-dimensional material attached to the target substrate.
Preferably, the production substrate comprises polydimethylsiloxane.
Preferably, the intercalation agent includes any one of absolute ethyl alcohol, deionized water or acetone.
Preferably, the intercalating agent is absolute ethanol.
As a preferred technical scheme of the invention, the selection of the intercalation agent needs to consider the cleanliness and the surface tension of the liquid, the intercalation agent with high cleanliness can be selected to avoid the two-dimensional material from being polluted by other impurity molecules, and the liquid with low surface tension can be selected to avoid the sample from being damaged. The invention preferably selects absolute ethyl alcohol as the intercalating agent with the best comprehensive effect, and if water is selected as the intercalating agent, the probability of damage of the two-dimensional material is higher due to higher surface tension of the water.
Preferably, the anhydrous ethanol is chromatographic grade anhydrous ethanol.
Preferably, the immersion time is 0.5-2 h, such as 0.7h, 0.9h, 1.1h, 1.3h, 1.5h or 1.7 h.
As a preferred technical scheme of the invention, the best wrinkle eliminating effect can be obtained by controlling the time for immersing the intercalation agent to be 0.5-2 h, and if the time for immersing is shorter than 0.5h, wrinkles are not completely eliminated; if the immersion time is longer than 2h, the surface of the two-dimensional material is contaminated by more impurity molecules.
Preferably, the annealing is preceded by a drying step.
Preferably, the drying method is nitrogen blow drying.
Preferably, the annealing treatment is performed in a quartz tube of a vacuum tube furnace.
Preferably, the annealing temperature is 100 to 300 ℃, for example, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃ or 280 ℃.
Preferably, the annealing treatment time is 1-3 h, such as 1.2h, 1.4h, 1.6h, 1.8h, 2h, 2.2h, 2.4h, 2.6h or 2.8 h.
Preferably, the annealing treatment is performed under protective gas conditions.
Preferably, the protective gas comprises hydrogen.
Preferably, the protective gas further comprises any one of nitrogen, helium or argon or a combination of at least two thereof.
As a preferred technical scheme, the method comprises the following steps:
(1) transferring the two-dimensional material mechanically stripped on the growth substrate to a target substrate to obtain a two-dimensional material attached to the target substrate;
(2) and (2) immersing the two-dimensional material attached to the target substrate obtained in the step (1) in an intercalation agent for 0.5-2 h, taking out, blowing and drying by using nitrogen, and annealing in a quartz tube of a vacuum tube furnace at the temperature of 100-300 ℃ for 1-3 h under the protection of protective gas to complete the removal of wrinkles of the two-dimensional material.
In a second aspect, the present invention provides a use of a method according to the first aspect for removing wrinkles in a two-dimensional material in an integrated device.
Compared with the prior art, the invention has the following beneficial effects:
the method for eliminating the two-dimensional material wrinkles comprises the steps of immersing a two-dimensional material attached to a target substrate into an intercalating agent, and carrying out annealing treatment to finish the elimination of the two-dimensional material wrinkles; the method for eliminating the wrinkles of the two-dimensional material not only has the advantages of simple operation and high efficiency, but also has the advantage of little influence on the self properties of the two-dimensional material; meanwhile, the method provided by the invention can eliminate the wrinkles of the two-dimensional material without special equipment and instruments in the operation process, has high elimination success rate and provides a new idea for realizing the nondestructive transfer of the two-dimensional material.
Drawings
Figure 1 is an atomic force microscope image of a double layer of molybdenum disulfide provided in example 1 prior to corrugation treatment;
figure 2 is an atomic force microscope image of the double layer molybdenum disulfide provided in example 1 after corrugation treatment;
fig. 3 is a normalized raman spectrum before and after the double-layer molybdenum disulfide corrugation treatment provided in example 1;
fig. 4 is an atomic force microscope image of three-layer graphene provided in example 2 before being wrinkled;
fig. 5 is an atomic force microscope image of three-layer graphene provided in example 2 after wrinkled treatment;
fig. 6 is a normalized raman spectrum before and after the three-layer graphene wrinkle treatment provided in example 2;
FIG. 7 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 3 before corrugation treatment;
figure 8 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 3 after corrugation treatment;
figure 9 is a normalized raman spectrum before and after treatment of a single layer molybdenum disulfide fold provided in example 3;
figure 10 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 4 prior to corrugation treatment;
figure 11 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 4 after corrugation treatment;
figure 12 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 5 prior to corrugation treatment;
figure 13 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 5 after corrugation treatment;
figure 14 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 6 prior to corrugation treatment;
figure 15 is an atomic force microscope image of a monolayer of molybdenum disulfide provided in example 6 after corrugation treatment.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
A method for eliminating double-layer molybdenum disulfide wrinkles specifically comprises the following steps:
(1) mechanically stripping double-layer (the thickness is about 1.3nm) molybdenum disulfide on dimethyl siloxane, and transferring the double-layer molybdenum disulfide to a silicon substrate by using a three-dimensional displacement table under an optical microscope to obtain a double-layer molybdenum disulfide sample attached to the silicon substrate;
(2) and (2) soaking the double-layer molybdenum disulfide sample attached to the silicon substrate obtained in the step (1) into chromatographic grade absolute ethyl alcohol for 1h by using tweezers (the cup mouth is sealed by using tin paper to prevent the absolute ethyl alcohol from evaporating), taking out the double-layer molybdenum disulfide sample attached to the silicon substrate by using the tweezers, blowing and drying by using nitrogen, and finally placing the double-layer molybdenum disulfide sample in a quartz tube of a vacuum tube furnace under the protection of a mixed gas of hydrogen and argon in a ratio of 1:9 for annealing treatment for 2h, wherein the annealing treatment temperature is 200 ℃, so that the double-layer molybdenum disulfide wrinkles are eliminated.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000071
Icon) to perform micro-area morphology observation on the double-layer molybdenum disulfide sample attached to the silicon substrate obtained in step (1) in this embodiment, an atomic force microscope image of the obtained double-layer molybdenum disulfide before wrinkle treatment is shown in fig. 1, and it can be seen from fig. 1 that the double-layer molybdenum disulfide attached to the silicon substrate has obvious wrinkles before treatment; using an atomic force microscope (Bruker)
Figure BDA0003589755980000072
Icon) performing micro-area morphology observation on the double-layer molybdenum disulfide sample attached to the silicon substrate after nitrogen blowing and drying in the step (2), wherein an atomic force microscope image of the double-layer molybdenum disulfide after fold treatment is obtained and is shown in fig. 2, and it can be seen from fig. 2 that the surface of the double-layer molybdenum disulfide attached to the silicon substrate after treatment becomes flat, and the existing folds are eliminated; in summary, the method provided by this embodiment can effectively eliminate the wrinkles of the double-layer molybdenum disulfide attached on the silicon substrate.
Using Raman spectrometer (
Figure BDA0003589755980000073
in Via Raman microscopy) on the double-layer molybdenum disulfide sample attached to the silicon substrate obtained in step (1) and the double-layer molybdenum disulfide attached to the silicon substrate after nitrogen blow drying in step (2)The molybdenum sulfide sample is tested, and the normalized raman spectrogram obtained by testing before and after the double-layer molybdenum disulfide wrinkling treatment is shown in fig. 3, and it can be seen from fig. 3 that the raman peaks of the double-layer molybdenum disulfide before and after the wrinkling treatment are basically overlapped, so that the method for eliminating the wrinkling provided by the embodiment does not cause doping or defects to the molybdenum disulfide.
Example 2
A method for wrinkling three-layer graphene specifically comprises the following steps:
(1) mechanically stripping three layers of graphene (the thickness is about 1.2nm) from dimethyl siloxane, and transferring the three layers of graphene to a silicon substrate by using a three-dimensional displacement platform under an optical microscope to obtain a three-layer graphene sample attached to the silicon substrate;
(2) and (2) immersing the three-layer graphene sample attached to the silicon substrate obtained in the step (1) into chromatographic grade absolute ethyl alcohol for 1h by using tweezers (the cup mouth is sealed by tin foil to prevent the absolute ethyl alcohol from evaporating), taking out the three-layer graphene sample attached to the silicon nitride substrate by using the tweezers, blowing and drying by using nitrogen, and finally placing the three-layer graphene sample in a quartz tube of a vacuum tube furnace for annealing treatment for 2h under the protection of a mixed gas of hydrogen and argon in a ratio of 1:9, wherein the annealing treatment temperature is 200 ℃, and the elimination of the three-layer graphene wrinkles is completed.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000081
Icon) performing micro-area morphology observation on the three-layer graphene sample attached to the silicon substrate obtained in the step (1) in the embodiment, wherein an atomic force microscope image before the three-layer graphene is subjected to wrinkle treatment is shown in fig. 4, and it can be seen from fig. 4 that obvious wrinkles exist on the surfaces of the three-layer graphene; using an atomic force microscope (Bruker)
Figure BDA0003589755980000082
Icon) micro-area morphology observation is carried out on the three-layer graphene attached to the silicon substrate after nitrogen blowing and drying in the step (2), and the atomic force microscope image of the three-layer graphene after fold processing is shown in fig. 5, which is obtained from fig. 5It can be seen that the three-layer graphene surface becomes flat and the pre-existing wrinkles have been eliminated; therefore, it can be seen that the method provided by the embodiment effectively eliminates the wrinkles of the three-layer graphene laminated on the silicon substrate.
Using Raman spectrometer (
Figure BDA0003589755980000083
in Via Raman Microscope) in this example, the three-layer graphene laminated on the silicon substrate obtained in step (1) and the three-layer graphene laminated on the silicon substrate after the nitrogen blow drying in step (2) were tested, and normalized Raman spectrograms before and after the three-layer graphene wrinkle treatment obtained by the test are shown in fig. 6, and it can be seen from fig. 6 that the normalized Raman spectrograms before and after the wrinkle treatment are located at about 1580cm-1Substantially coincide and are after treatment at about 1350cm-1No defect peak D appears at the position, which shows that the fold treatment does not cause defects to the graphene.
Example 3
A method for eliminating folds of a single layer of molybdenum disulfide comprises the following steps:
(1) mechanically stripping molybdenum disulfide containing a single layer (the thickness of each layer is about 0.65nm) from dimethyl siloxane, and transferring the single layer of molybdenum disulfide to a silicon nitride substrate with holes by using a three-dimensional displacement platform under an optical microscope to obtain a suspended single layer of molybdenum disulfide sample attached to the silicon nitride substrate;
(2) and (2) immersing the suspended monolayer molybdenum disulfide attached to the silicon nitride substrate obtained in the step (1) into chromatographic grade absolute ethyl alcohol for 1h by using tweezers (the cup mouth is sealed by tin paper to prevent the absolute ethyl alcohol from evaporating), taking out the suspended monolayer molybdenum disulfide on the silicon nitride substrate by using the tweezers, blowing and drying by using nitrogen, and finally placing the silicon nitride substrate in a quartz tube of a vacuum tube furnace under the protection of a mixed gas of hydrogen and argon in a ratio of 1:9 for annealing treatment for 2h, wherein the annealing treatment temperature is 200 ℃, so that the elimination of the monolayer molybdenum disulfide wrinkles is completed.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000091
Icon) performing micro-area morphology observation on the suspended monolayer molybdenum disulfide attached to the silicon nitride substrate obtained in the step (1) in the embodiment, wherein an atomic force microscope image of the suspended monolayer molybdenum disulfide before wrinkle treatment is shown in fig. 7, and it can be seen from fig. 7 that obvious wrinkles exist in the monolayer molybdenum disulfide in the suspended region; using an atomic force microscope (Bruker)
Figure BDA0003589755980000092
Icon) performing micro-area morphology observation on the suspended molybdenum disulfide attached to the silicon nitride substrate after nitrogen blowing and drying in the step (2), wherein an atomic force microscope image of the molybdenum disulfide subjected to wrinkle treatment is shown in fig. 8, and it can be seen from fig. 8 that a single layer of molybdenum disulfide at a suspended area becomes flat, and the existing wrinkles are eliminated; therefore, it can be seen that the method provided by the embodiment effectively eliminates wrinkles of the suspended monolayer of molybdenum disulfide attached to the silicon nitride substrate.
Using Raman spectrometer (
Figure BDA0003589755980000093
inVia Raman Microscope) tests the suspended molybdenum disulfide on the bonded silicon nitride substrate obtained in the step (1) and the suspended molybdenum disulfide on the silicon nitride substrate subjected to nitrogen blow drying in the step (2), and normalized Raman spectrograms of the suspended molybdenum disulfide before and after single-layer molybdenum disulfide wrinkle treatment in the obtained test are shown in fig. 9, and it can be seen from fig. 9 that Raman peaks of the single-layer molybdenum disulfide before and after the wrinkle treatment are basically coincident, which indicates that the wrinkle treatment does not cause doping or defects to the molybdenum disulfide.
Example 4
A method for eliminating wrinkles of a monolayer of molybdenum disulfide is different from the method in example 3 only in that the immersion time in absolute ethyl alcohol is 15min, and other conditions, parameters and steps are the same as those in example 3.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000101
Icon) bonded silicon nitride obtained in example 4Micro-area morphology observation is carried out on the suspended molybdenum disulfide on the substrate, an atomic force microscope image of the single-layer molybdenum disulfide before wrinkling treatment is shown in fig. 10, and it can be seen from fig. 10 that obvious wrinkles exist in the single-layer molybdenum disulfide at the suspended area; using an atomic force microscope (Bruker)
Figure BDA0003589755980000102
Icon) performing micro-area morphology observation on the suspended molybdenum disulfide attached to the silicon nitride substrate after nitrogen blowing and drying, wherein an atomic force microscope image of the molybdenum disulfide subjected to wrinkle treatment is shown in fig. 11, and it can be seen from fig. 11 that a part of wrinkles still exist in a single-layer molybdenum disulfide layer in a suspension region and are not eliminated; therefore, it can be said that the immersion time is too short and the wrinkle structure is not effectively completely eliminated.
Example 5
A method for eliminating wrinkles of a monolayer of molybdenum disulfide is different from the method in the embodiment 3 only in that the immersion time of the molybdenum disulfide monolayer in absolute ethyl alcohol is 5 hours, and other conditions, parameters and steps are the same as the embodiment 3.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000103
Icon) micro-area morphology observation is carried out on the suspended monolayer molybdenum disulfide attached to the silicon nitride substrate obtained in the embodiment 5, an atomic force microscope image of the suspended monolayer molybdenum disulfide before wrinkle treatment is shown in fig. 12, and it can be seen from fig. 12 that obvious wrinkles exist in the monolayer molybdenum disulfide in the suspended area; using an atomic force microscope (Bruker)
Figure BDA0003589755980000104
Icon) performing micro-area morphology observation on the suspended single-layer molybdenum disulfide attached to the silicon nitride substrate after nitrogen blowing and drying, wherein an atomic force microscope image of the molybdenum disulfide subjected to wrinkle treatment is shown in fig. 13, and it can be seen from fig. 13 that the single-layer molybdenum disulfide wrinkles at the suspended area are eliminated, but a large amount of impurities are accumulated on the surface of the molybdenum disulfide; thus, it can be stated that the immersion time is too long, and although the wrinkle structure can be eliminated, it is still possible toThe soaking time is too long, so that impurity molecules are accumulated on the surface of the molybdenum disulfide, and the sample is polluted.
Example 6
A method for removing wrinkles from a monolayer of molybdenum disulfide, which is different from example 3 only in that deionized water is used to replace chromatographic grade absolute ethyl alcohol, and other conditions, parameters and steps are the same as those in example 3.
Using an atomic force microscope (Bruker)
Figure BDA0003589755980000111
Icon) performing micro-area morphology observation on the suspended molybdenum disulfide attached to the silicon nitride substrate obtained in the step (1) in the embodiment, wherein an atomic force microscope image of the obtained single-layer molybdenum disulfide before wrinkle treatment is shown in fig. 14, and it can be seen from fig. 14 that obvious wrinkles exist in the single-layer molybdenum disulfide at the suspension region; using an atomic force microscope (Bruker)
Figure BDA0003589755980000112
Icon) micro-area morphology observation is carried out on the suspended molybdenum disulfide attached to the silicon nitride substrate after nitrogen blowing and drying in the step (2), an atomic force microscope image of the molybdenum disulfide after fold treatment is shown in fig. 15, the morphology of a single-layer suspensible sample in fig. 15 is changed greatly, and the sample at a hole is damaged; therefore, it can be seen that the method provided by this embodiment damages the suspended monolayer of molybdenum disulfide by using deionized water with a higher surface tension.
In conclusion, the two-dimensional material wrinkles can be effectively eliminated by the two-dimensional material wrinkles eliminating methods provided by embodiments 1 to 6, and the success rate is high. By comparing example 3 with examples 4 to 5, it can be seen that the time for immersing the intercalating agent is within the range defined in the present application, which results in the best effect of the elimination; and it can be found by comparing example 3 with example 6 that anhydrous ethanol as an intercalating agent is more advantageous for eliminating wrinkles of the two-dimensional material than water as an intercalating agent, and does not damage the performance of the two-dimensional material itself.
The applicant states that the present invention describes a method for removing wrinkles from a two-dimensional material and an application thereof through the above embodiments, but the present invention is not limited to the above process steps, i.e. it does not mean that the present invention must rely on the above process steps to be implemented. It will be apparent to those skilled in the art that any modifications to the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific forms, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. A method of de-wrinkling a two-dimensional material, the method comprising: and (3) immersing the two-dimensional material attached to the target substrate into an intercalation agent, and performing annealing treatment to finish the elimination of the wrinkles of the two-dimensional material.
2. The method of claim 1, wherein the two-dimensional material comprises any one of graphene, graphene oxide, hexagonal boron nitride, or a transition metal chalcogenide;
preferably, the transition metal chalcogenide compound includes any one of molybdenum disulfide, molybdenum diselenide, or tungsten diselenide;
preferably, the thickness of the two-dimensional material is 0.3-30 nm.
3. The method of claim 1 or 2, wherein the target substrate comprises a silicon substrate or a silicon nitride substrate.
4. The method according to any one of claims 1 to 3, wherein the two-dimensional material attached to the target substrate is prepared by a method comprising: transferring the two-dimensional material mechanically stripped on the growth substrate to a target substrate to obtain the two-dimensional material attached to the target substrate;
preferably, the growth substrate comprises polydimethylsiloxane.
5. The method of any of claims 1 to 4, wherein the intercalating agent comprises any of absolute ethanol, deionized water or acetone;
preferably, the intercalant comprises absolute ethanol;
preferably, the anhydrous ethanol is chromatographic grade anhydrous ethanol.
6. The method according to any one of claims 1 to 5, wherein the immersion time is 0.5 to 2 hours.
7. The method according to any one of claims 1 to 6, further comprising a step of drying before the annealing;
preferably, the drying method is nitrogen blow drying.
8. The method according to any one of claims 1 to 7, wherein the annealing treatment is performed in a quartz tube of a vacuum tube furnace;
preferably, the temperature of the annealing treatment is 100-300 ℃;
preferably, the annealing treatment time is 1-3 h;
preferably, the annealing treatment is performed under protective gas conditions;
preferably, the protective gas comprises hydrogen;
preferably, the protective gas further comprises any one or a combination of at least two of nitrogen, helium or argon.
9. A method according to any one of claims 1 to 8, characterized in that the method comprises the steps of:
(1) transferring the two-dimensional material mechanically stripped on the growth substrate to a target substrate to obtain a two-dimensional material attached to the target substrate;
(2) and (2) immersing the two-dimensional material attached to the target substrate obtained in the step (1) in an intercalation agent for 0.5-2 h, taking out, blowing and drying by using nitrogen, and annealing in a quartz tube of a vacuum tube furnace at the temperature of 100-300 ℃ for 1-3 h under the protection of protective gas to complete the removal of wrinkles of the two-dimensional material.
10. Use of a method of de-wrinkling a two-dimensional material according to any one of claims 1 to 9 in an integrated device.
CN202210374537.9A 2022-04-11 2022-04-11 Method for eliminating two-dimensional material wrinkles and application thereof Pending CN114772547A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210374537.9A CN114772547A (en) 2022-04-11 2022-04-11 Method for eliminating two-dimensional material wrinkles and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210374537.9A CN114772547A (en) 2022-04-11 2022-04-11 Method for eliminating two-dimensional material wrinkles and application thereof

Publications (1)

Publication Number Publication Date
CN114772547A true CN114772547A (en) 2022-07-22

Family

ID=82429898

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210374537.9A Pending CN114772547A (en) 2022-04-11 2022-04-11 Method for eliminating two-dimensional material wrinkles and application thereof

Country Status (1)

Country Link
CN (1) CN114772547A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102903631A (en) * 2012-10-22 2013-01-30 西安电子科技大学 Annealing technology for transferring graphene by GaN substrate and device manufactured thereby
CN102931078A (en) * 2012-10-22 2013-02-13 西安电子科技大学 Annealing method of sapphire substrate transfer graphene
US20200083037A1 (en) * 2016-07-08 2020-03-12 Cornell University Transition metal chalcogenide van der waals films, methods of making same, and apparatuses and devices comprising same
CN112768345A (en) * 2021-01-11 2021-05-07 山东理工大学 Preparation method of two-dimensional heterojunction based on graphene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102903631A (en) * 2012-10-22 2013-01-30 西安电子科技大学 Annealing technology for transferring graphene by GaN substrate and device manufactured thereby
CN102931078A (en) * 2012-10-22 2013-02-13 西安电子科技大学 Annealing method of sapphire substrate transfer graphene
US20200083037A1 (en) * 2016-07-08 2020-03-12 Cornell University Transition metal chalcogenide van der waals films, methods of making same, and apparatuses and devices comprising same
CN112768345A (en) * 2021-01-11 2021-05-07 山东理工大学 Preparation method of two-dimensional heterojunction based on graphene

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
HONGHWI PARK 等: "Optimized poly(methyl methacrylate)-mediated graphene-transfer process for fabrication of high-quality graphene layer", NANOTECHNOLOGY, vol. 29, pages 415303, XP020331190, DOI: 10.1088/1361-6528/aad4d9 *
WEI DAWEI 等: "Friction of MoO3 Nanoflakes on Graphite Surface with an Ace-like Intercalation Layer", CHEM. RES. CHINESE UNIVERSITIES, vol. 38, no. 3, pages 769 - 773 *
张光杰 等: "柔性压电纳米发电机研究进展", 新材料产业, pages 58 - 63 *

Similar Documents

Publication Publication Date Title
US11760641B2 (en) Method for manufacturing suspended graphene support film by selectively etching growth substrate
Hong et al. A rational strategy for graphene transfer on substrates with rough features
Bao et al. Lithography-free fabrication of high quality substrate-supported and freestanding graphene devices
Pankove et al. Hydrogenation and dehydrogenation of amorphous and crystalline silicon
US9087692B2 (en) Method for transferring a graphene layer
JP5872557B2 (en) Large-scale graphene sheet, article incorporating the same, composition, method and apparatus
US10272647B2 (en) Graphene and polymer-free method for transferring CVD grown graphene onto hydrophobic substrates
KR20140121137A (en) Method and board for growing high quality graphene layer using high pressure annealing
Xu et al. Direct bonding of silicon and quartz glass using VUV/O3 activation and a multistep low-temperature annealing process
US9895870B2 (en) Graphene surface functionality transfer
CN108069416B (en) Ultra-clean graphene and preparation method thereof
CN108871890B (en) Method for preparing TEM sample by using graphene as protective layer
Gui et al. Effects of substrates on Raman spectroscopy in chemical vapor deposition grown graphene transferred with poly (methyl methacrylate)
CN109321893B (en) Preparation method of graphene protective film, graphene protective film and use method thereof
CN114772547A (en) Method for eliminating two-dimensional material wrinkles and application thereof
CN113023718A (en) Method for preparing high-quality suspended two-dimensional material support film through clean transfer
TWI679167B (en) Method of Transferring Two-dimensional Nanomaterials with Carbon Nanotube Composite Film
TW201509795A (en) Method of transferring graphene layer
Ding et al. Direct observation of the strong interaction between carbon nanotubes and quartz substrate
CN114394589B (en) Method for transferring strain graphene on silicon substrate containing oxide layer
CN113421826B (en) Atomic-level precision lossless layer-by-layer etching method for two-dimensional layered material
CN114171370A (en) Method for preparing graphene in relatively closed area by solid phase method
TW201939567A (en) Transmission electron microscope micro-grid and method for manufacturing the same
CN109839392B (en) Self-supporting thin film transmission electron microscope sample and preparation method thereof
Kolari et al. Smoothing of microfabricated silicon features by thermal annealing in reducing or inert atmospheres

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination