CN111704128B - Two-dimensional material transfer method based on substrate with steps - Google Patents
Two-dimensional material transfer method based on substrate with steps Download PDFInfo
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- CN111704128B CN111704128B CN202010458450.0A CN202010458450A CN111704128B CN 111704128 B CN111704128 B CN 111704128B CN 202010458450 A CN202010458450 A CN 202010458450A CN 111704128 B CN111704128 B CN 111704128B
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Abstract
The invention discloses a two-dimensional material transfer method based on a substrate with steps, which comprises the following steps: manufacturing a two-dimensional material layer on a substrate, spin-coating PMMA, manufacturing PDMS/PMMA/two-dimensional material/substrate, etching silicon oxide on the substrate, releasing the PDMS/PMMA/two-dimensional material, combining the two-dimensional material to be transferred with a target substrate, and dissolving PMMA. The transfer method is suitable for flattening the substrate and the substrate with steps caused by adding electrodes and the like; meanwhile, a method of direct wet etching by using a sodium hydroxide solution is adopted, so that a two-dimensional material, particularly graphene, is prevented from curling in the transfer process, the transfer success rate is improved, and the cost is reduced; the isopropanol is used for cleaning the two-dimensional material after the silicon oxide is etched instead of the deionized water, firstly, the isopropanol is volatile, and secondly, when the two-dimensional material is combined with a target substrate and PMMA is etched, the isopropanol can increase the combination force of the two-dimensional material and the substrate, so that the two-dimensional material cannot be curled and deviated.
Description
Technical Field
The invention relates to the technical field of material transfer, in particular to a two-dimensional material transfer method based on a substrate with steps.
Background
The two-dimensional material commonly used at present comprises graphene, molybdenum disulfide, tungsten disulfide, boron nitride and the like, and after the graphene is found for the first time in 2004, the research and application development of the two-dimensional material are rapid, and the two-dimensional material has wide application prospects in the fields of biological detection, microelectronics and the like. At present, the main methods for preparing the two-dimensional material comprise a mechanical stripping method, a chemical oxidation-reduction method and a gas image deposition method, wherein the mechanical stripping method is the main method for preparing a two-dimensional material sample by generally carrying out experimental research, and compared with other methods, the quality of the prepared single crystal thin-layer two-dimensional material is higher. In either fabrication method, the two-dimensional material is then transferred to a target substrate to complete subsequent experiments. However, the currently widely used wet and dry transfer methods are both to transfer two-dimensional materials onto flat substrates such as silicon nitride, silicon oxide, etc. When the substrate is not flat due to the presence of electrodes (or other steps) on the surface of the target substrate, these conventional methods may not be able to transfer to a specified location due to the reduced contact area of the two-dimensional material with the substrate.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects of the background art, the invention provides a two-dimensional material transfer method based on a stepped substrate, which can transfer a two-dimensional material to a specified position of a stepped target substrate at a fixed point without damaging the target substrate.
The technical scheme is as follows: the invention discloses a two-dimensional material transfer method based on a substrate with steps, which comprises the following steps of:
s1, peeling the two-dimensional material to be transferred off the silicon oxide/silicon substrate to form a two-dimensional material layer, and spin-coating PMMA on the two-dimensional material layer to form a two-dimensional material/PMMA layer;
s2, pressing the two-dimensional material/PMMA layer onto the punched PDMS block, wherein the two-dimensional material is positioned in the center of the hole;
s3, placing the sample obtained in the S2 in a sodium hydroxide solution to etch silicon oxide, and releasing a two-dimensional material/PMMA/PDMS;
s4, putting the two-dimensional material/PMMA/PDMS into isopropanol solution for cleaning, and then aligning the two-dimensional material to a target position on a target substrate for compressing;
s5, the sample obtained in S4 is placed in an acetone solution to dissolve PMMA, namely, the two-dimensional material is successfully transferred to the accurate position of the target substrate.
The two-dimensional material to be transferred is graphene. Other two-dimensional materials such as molybdenum disulfide and boron nitride can also be transferred.
Further, in S1, the two-dimensional material to be transferred may be peeled off from the PMMA and then pressed onto the silicon oxide/silicon substrate.
Further, in S1, the PMMA is spin-coated for 2-3 times, and the thickness of the PMMA film is guaranteed to be 0.5-0.8 microns.
Furthermore, the PDMS block in S2 is punched by a cylindrical puncher, the aperture is 2-3 mm, the difficulty of searching for the two-dimensional material can be reduced in the later processing, and the refraction and reflection of PDMS to the microscope laser can be removed, so that the imaging of the two-dimensional material is clearer.
Further, the mass fraction of the sodium hydroxide solution in S3 is 30% to 35%, too high results in material waste, and too low reduces the etching rate.
Has the advantages that: compared with the prior art, the invention has the advantages that: firstly, the transfer method is suitable for flattening the substrate and the substrate with steps caused by adding electrodes and the like; secondly, a method of direct wet etching by using a sodium hydroxide solution is adopted, so that a two-dimensional material, particularly graphene, is prevented from curling in the transfer process, the transfer success rate is improved, and the cost is reduced; meanwhile, the isopropanol is used for cleaning the two-dimensional material after silicon oxide etching instead of deionized water, firstly, the isopropanol is volatile, and secondly, when the two-dimensional material is combined with a target substrate and PMMA is etched, the isopropanol can increase the combination force of the two-dimensional material and the substrate, so that the two-dimensional material cannot be curled and deflected.
Drawings
FIG. 1 is a schematic view of the transfer process of the present invention;
fig. 2 is a graph of transfer results of graphene in the example.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples.
Example 1
The two-dimensional material transfer method based on the substrate with the step as shown in fig. 1 includes a two-dimensional material preparation and transfer process, the two-dimensional material preparation adopts a mechanical peeling method, the transfer adopts an improved wet transfer method, and the two-dimensional material to be transferred adopts graphene in this embodiment.
The method specifically comprises the following steps:
(1) stripping graphene on a silicon oxide/silicon substrate to form a graphene layer, preferably the silicon oxide/silicon substrate with the thickness of 285 nm silicon oxide, spin-coating a PMMA anisole solution with the mass fraction of 4% on the graphene layer, and spin-coating for 2 times to ensure that the thickness of the PMMA film is 0.5 micron.
Graphene can also be exfoliated onto PMMA before it is pressed onto the silicon oxide/silicon substrate.
(2) The method comprises the following steps of pressing a graphene/PMMA layer onto a perforated PDMS square under an optical microscope, wherein the graphene is located in the center of a hole, the PDMS is easy to adhere to the PMMA due to the high viscosity of the PDMS, and the PMMA, the graphene and a substrate have strong van der Waals force and cannot cause the graphene to fall off; if the PDMS is directly contacted with the graphene layer, the transfer fails due to weak bonding force between the PDMS and the graphene, and thus the object of the present invention is not achieved.
Adopt cylindrical hole puncher, the hole diameter is 2 millimeters, can reduce the degree of difficulty of looking for the two-dimensional material in later stage processing, can also get rid of PDMS to the refraction and the reflection of microscope laser, makes the two-dimensional material formation of image more clear.
The PDMS thickness was 3 mm. When the thickness of PDMS is too low, the strength of PDMS is too low, which is not favorable for the transfer process.
(3) Putting the obtained whole sample into a sodium hydroxide solution to etch silicon oxide so as to release graphene/PMMA/PDMS; the mass fraction of the sodium hydroxide solution is 30 percent.
(4) The method comprises the steps of fishing out graphene/PMMA/PDMS, putting the graphene/PMMA/PDMS into an isopropanol solution for cleaning, then fishing out the graphene/PDMS to align the graphene at a target position, and then pressing the graphene and a target substrate tightly, wherein in order to transfer the graphene to the accurate position of the substrate, the process needs to be operated under an optical microscope.
The method for searching the graphene film under the optical microscope comprises the following steps: firstly, finding a hole area on PDMS under a 10-time lens, then directly finding graphene in the center area of the hole, and finally, changing a lens to a 50-time lens to amplify the graphene so as to perform subsequent operation.
And (5) performing the operations of the step (2) and the step (4) under an optical microscope to accurately position the positions of the graphene and the target substrate.
(5) And finally, placing the substrate in an acetone solution to dissolve PMMA, and after dissolution, taking the substrate under an optical microscope to observe whether the transfer is successful or not, wherein a Raman spectrum test can also be used.
As shown in fig. 2, a graph of the result of graphene transfer in this embodiment includes, from top to bottom, a graphene layer 1, a step 2 (electrode), a silicon nitride film 3 and a silicon substrate 4. The graphene is required to be in contact with electrodes at two ends, and can completely cover the small holes in the silicon nitride film. If dry transfer is used, this can lead to damage of the steps (electrodes) and thus destruction of the entire substrate. Therefore, wet transfer is used, and the PMMA is etched by acetone in the last step, so that the graphene is separated from the PMMA/PDMS layer and is successfully transferred to the target position of the substrate.
Example 2
The invention relates to a two-dimensional material transfer method based on a substrate with steps, which specifically comprises the following steps:
(1) stripping graphene on a silicon oxide/silicon substrate to form a graphene layer, spin-coating PMMA on the graphene layer for 2 times, and ensuring that the thickness of a PMMA film is 0.65 micron;
(2) pressing a graphene/PMMA layer onto a perforated PDMS square under an optical microscope, wherein the graphene is positioned in the center of a hole; a cylindrical punch was used, with a hole diameter of 2.5 mm.
(3) Putting the obtained whole sample into a sodium hydroxide solution to etch silicon oxide so as to release graphene/PMMA/PDMS; the mass fraction of the sodium hydroxide solution was 33%.
(4) And fishing out the graphene/PMMA/PDMS, putting the graphene/PMMA/PDMS into an isopropanol solution for cleaning, fishing out the graphene/PMMA/PDMS to align the graphene to a target position, and then pressing the graphene and the target substrate tightly.
(5) Finally, the PMMA was dissolved in acetone solution.
Example 3
The invention relates to a two-dimensional material transfer method based on a substrate with steps, which specifically comprises the following steps:
(1) stripping graphene on a silicon oxide/silicon substrate to form a graphene layer, spin-coating PMMA on the graphene layer for 3 times to ensure that the thickness of a PMMA film is 0.8 micron;
(2) compressing a graphene/PMMA layer onto a perforated PDMS square under an optical microscope, wherein the graphene is positioned in the center of a hole; a cylindrical punch was used, the hole diameter being 3 mm.
(3) Putting the obtained whole sample into a sodium hydroxide solution to etch silicon oxide so as to release graphene/PMMA/PDMS; the mass fraction of the sodium hydroxide solution is 35 percent.
(4) And fishing out the graphene/PMMA/PDMS, putting the graphene/PMMA/PDMS into an isopropanol solution for cleaning, fishing out the graphene/PMMA/PDMS to align the graphene to a target position, and then pressing the graphene and the target substrate tightly.
(5) Finally, the PMMA was dissolved in acetone solution.
Claims (1)
1. A two-dimensional material transfer method based on a substrate with steps is characterized by comprising the following steps:
s1, peeling the two-dimensional material to be transferred on the silicon oxide/silicon substrate to form a two-dimensional material layer, and spin-coating PMMA on the two-dimensional material layer to form a two-dimensional material/PMMA layer, or peeling the two-dimensional material to be transferred on the PMMA first and then pressing the two-dimensional material on the silicon oxide/silicon substrate;
s2, pressing the two-dimensional material/PMMA layer onto the perforated PDMS block, wherein the two-dimensional material is located in the center of the hole;
s3, placing the sample obtained in the S2 in a sodium hydroxide solution to etch silicon oxide, and releasing a two-dimensional material/PMMA/PDMS;
s4, putting the two-dimensional material/PMMA/PDMS into isopropanol solution for cleaning, and then aligning the two-dimensional material to a target position on a target substrate for compressing;
s5, placing the sample obtained in the step S4 in an acetone solution to dissolve PMMA, namely successfully transferring the two-dimensional material to the accurate position of the target substrate;
The two-dimensional material to be transferred adopts graphene;
spin-coating PMMA for 2-3 times in S1 to ensure that the thickness of a PMMA film is 0.5-0.8 micron;
in the S2, punching a PDMS block by using a cylindrical puncher, wherein the aperture is 2-3 mm;
the mass fraction of the sodium hydroxide solution in the S3 is 30-35%.
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| CN114920239B (en) * | 2022-05-10 | 2023-10-20 | 北京理工大学 | Two-dimensional material transferring or stacking method based on water vapor |
| CN115650295A (en) * | 2022-09-28 | 2023-01-31 | 浙江大学杭州国际科创中心 | Transfer method of thin-layer two-dimensional material |
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