CN116462155A - Method for constructing multilayer two-dimensional layered material based on PVA film - Google Patents
Method for constructing multilayer two-dimensional layered material based on PVA film Download PDFInfo
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- CN116462155A CN116462155A CN202310482381.0A CN202310482381A CN116462155A CN 116462155 A CN116462155 A CN 116462155A CN 202310482381 A CN202310482381 A CN 202310482381A CN 116462155 A CN116462155 A CN 116462155A
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000012546 transfer Methods 0.000 claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 60
- 229910052710 silicon Inorganic materials 0.000 claims description 60
- 239000010703 silicon Substances 0.000 claims description 60
- 238000010438 heat treatment Methods 0.000 claims description 36
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 31
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 31
- 239000011521 glass Substances 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002390 adhesive tape Substances 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000008213 purified water Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims 5
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 5
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims 5
- 238000000861 blow drying Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 69
- 229920002451 polyvinyl alcohol Polymers 0.000 description 69
- 239000010410 layer Substances 0.000 description 15
- 238000001035 drying Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052582 BN Inorganic materials 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- -1 polypropylene carbonate Polymers 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 2
- WCQOLGZNMNEYDX-UHFFFAOYSA-N bis(selanylidene)vanadium Chemical compound [Se]=[V]=[Se] WCQOLGZNMNEYDX-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920000379 polypropylene carbonate Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
- B81C2201/0191—Transfer of a layer from a carrier wafer to a device wafer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/05—Temporary protection of devices or parts of the devices during manufacturing
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A method for constructing a multilayer two-dimensional layered material based on a PVA film comprises the steps of preparing a PVA solution; preparing a PVA film; constructing a two-dimensional layered material torsion homogeneous structure and a heterostructure; transferring the two-dimensional heterostructure to a target substrate, and the like. The invention has the following technical effects: (1) The water solubility of the PVA film ensures that the material interface can not introduce pollution and has little damage to the sample; (2) The PVA has high viscosity enough to divide the same sheet material into two parts, so that the position and the original structural arrangement orientation of the material can be accurately controlled in the transfer process, and the requirements of preparation and the like of a torsion angle homogeneous structure, a heterostructure and the like are met; (3) The transfer scheme with high flexibility, high efficiency, simplicity, no damage and low cost is provided for the two-dimensional layered material.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a high-efficiency transfer method for two-dimensional layered material stacking.
Background
The two-dimensional layered material is a crystal plane structure held together by strong in-plane covalent bonds and weak out-of-plane van der Waals forces, and each monolayer can be detached from the bulk by mechanical exfoliation to overcome van der Waals forces and maintain a high quality crystal structure. The heterojunction constructed by the two-dimensional layered material has the characteristics of clean interface and no limitation of lattice matching, is convenient for researchers to design a large number of samples with excellent performance, and brings infinite possibility for electronic devices.
In the van der Waals layered structure, the torsion angle between two-dimensional layered materials is an extra degree of freedom, and structures with different properties can be obtained by adjusting the angle between two atomic lattices, so that researchers can design a large number of combinations of van der Waals materials. In order to have a twist angle stack, the structural arrangement of the materials to be stacked needs to be known, and the simplest is to divide the same two-dimensional layered material into different parts for translation, and apply the twist angle stack to form van der Waals homojunctions with the twist angle.
The traditional mechanical stripping method uses films such as polymethyl methacrylate (PMMA), polypropylene carbonate (PPC), polycarbonate (PC), polydimethylsiloxane (PDMS) and the like as a transfer medium layer, and has the problems of too high temperature requirement, introduction of pollution elements and the like. The most commonly used dry transfer is to repeatedly peel off the adhesive tape to obtain a few-layer sample, then tear the few-layer sample on PDMS to obtain a required thin-layer sample, and finally transfer the thin-layer sample to a target substrate. The problem with this method is that the adhesion between the different materials and the different substrates is different, and the viscosity of the PDMS is poorly controlled during the transfer of the sample from the PDMS to the substrates. Particularly in the case of preparing the homo/heterojunction, if the adhesion between the material and PDMS is greater than that between the materials, the transfer process is extremely difficult and the sample is easily broken. And the PDMS is easy to remain residual glue on the surface of the sample in the transfer process, so that the sample is polluted. In addition, samples transferred through PDMS are difficult to pick up, resulting in low flexibility in building a multi-layer heterostructure. Polyvinyl alcohol (PVA) is used as a water-soluble film, has strong adhesive force to a two-dimensional layered material after temperature rising, can control the viscosity of the two-dimensional layered material by controlling the temperature, has small water-soluble pollution, and has obvious advantages compared with other methods for preparing a multi-layer two-dimensional structure.
Disclosure of Invention
The invention aims to provide a method for constructing a multi-layer two-dimensional layered material based on a PVA film, which has the characteristics of simplicity, convenience, no pollution, low operation difficulty and flexible transfer, and can achieve the purpose of constructing a multi-layer two-dimensional layered heterostructure and a homogeneous structure with torsion angles in a lossless, rapid and effective manner.
The invention is realized by the following technical scheme.
The invention relates to a method for constructing a multilayer two-dimensional layered material based on a PVA film, which comprises the following steps.
Step 1: preparation of PVA solution.
a. Adding 88000 molecular weight PVA particles into a clean container, adding a proper amount of purified water, and ensuring that the final solution quality concentration is controlled to be 2% -5%, wherein insufficient dissolution can be caused by too high concentration, and the viscosity of the film can be reduced by too low concentration.
b. The container is placed on a magnetic heating table, heated and stirred until PVA is completely dissolved, the solution is transparent and bubble-free, and the solution is stored in a sealed manner at normal temperature and is kept stand.
Step 2: preparation of PVA film.
A piece of PDMS film is cut and stuck on a clean glass slide, PVA solution is absorbed by a liquid-transferring gun and is dripped on the PDMS film, PVA liquid drops are scraped by the tip of the liquid-transferring gun to uniformly wet the PDMS, then the glass slide is placed on a heating table, the glass slide is heated at 60 ℃ for at least 5 minutes, and after moisture is evaporated, the PVA film with the thickness of micron level and transparent and uniform is finally formed on the PDMS film.
Step 3: and constructing a two-dimensional layered material heterostructure.
a. And sequentially carrying out three ultrasonic cleaning on the silicon wafer by acetone, isopropanol and deionized water to remove impurities on the surface of the silicon wafer, and drying the surface moisture by a nitrogen gun.
b. And repeatedly stripping the preferred parent material by using an adhesive tape, attaching the parent material to the cleaned silicon wafer, and finding the target layered material I to be transferred by using a microscope.
c. And (3) fixing the silicon wafer processed in the step (3 b) on a transfer table, inversely fixing the glass slide obtained in the step (2) on a mechanical arm of the transfer table, and enabling one side of the PVA film to face the silicon wafer. Operating a microscope of a transfer table to focus the target layered material I to be transferred on a silicon wafer, and controlling a mechanical arm to move horizontally so that the PVA film completely covers the target layered material I; and controlling the mechanical arm to move in the vertical direction, and attaching the glass slide to the silicon wafer, so that the PVA film is completely attached to the target layered material I.
d. And fixing the mechanical arm of the transfer table, opening the heating table to heat up to 75 ℃, maintaining for 20 seconds, and stopping heating. After the silicon wafer is cooled to below 40 ℃, the PVA film is solidified, the mechanical arm is lifted, and at the moment, the target sample I is stuck by the PVA film and lifted along with the glass slide.
e. And (3) replacing the parent material, repeatedly dissociating by using an adhesive tape, attaching the parent material to a silicon wafer subjected to three ultrasonic cleaning processes of acetone, isopropanol and deionized water, finding a target layered material II to be transferred by using a microscope, and replacing the silicon wafer on the transfer platform with the silicon wafer with the target layered material II. And (3) operating the transfer table microscope to focus the transfer table microscope on the target layered material II to be transferred, controlling the mechanical arm to move so that the two samples are aligned to the desired positions, and lowering the mechanical arm to tightly attach the glass slide and the silicon wafer to form a two-dimensional heterostructure. The heating table was turned on to raise the temperature to 75℃and after maintaining for 20 seconds, the heating was stopped. And after the silicon wafer is cooled to below 40 ℃ and the PVA film is solidified, the mechanical arm is lifted, the two-dimensional heterostructure is lifted, and the whole structure is shown in figure 1.
Step 4: transferring the two-dimensional heterostructure onto a target substrate.
a. On the basis of the step 3e, the replacement target substrate is fixed on a transfer table, a mechanical arm of the transfer table is controlled to descend, the two-dimensional heterostructure is aligned to the target substrate in the descending process, and the glass slide is tightly attached to the substrate. The heating table is opened, the temperature is raised to 90 ℃ for 20s, the mechanical arm is slowly lifted, the PVA film can be separated from the PDMS film, and the PVA film is left on the target substrate.
b. Placing the substrate with the two-dimensional heterostructure and the PVA film into purified water, heating to 80 ℃, completely dissolving the PVA film after 30 minutes, removing the substrate, lightly blowing by using a helium gun to remove surface moisture, and completing the construction process by means of the two-dimensional layered material heterostructure of the PVA film.
Step 3 of the present invention may be repeated multiple times to stack the same or different materials, or the same sample may be torn with PVA to apply a twist angle stack to form a multilayer two-dimensional heterostructure or a homostructure with twist angles.
The advantages of the present invention compared to conventional methods are as follows.
(1) The water solubility of the PVA film used in the invention ensures that the material interface does not introduce pollution and has little damage to the sample.
(2) The PVA has high viscosity enough to divide the same sheet material into two parts, so that the position and the original structural arrangement orientation of the material can be accurately controlled in the transfer process, and the requirements of preparation of a torsion angle homogeneous structure, a heterostructure and the like are met.
(3) The invention provides a transfer scheme with high flexibility, high efficiency, simplicity, no damage and low cost for the two-dimensional layered material.
Drawings
Fig. 1 is a schematic diagram of the final structure after the completion of step 3 of the present invention. 1 is a glass slide, 2 is a PDMS film, 3 is a PVA film, 4 is a target two-dimensional layered material I, and 5 is a target two-dimensional layered material II.
Fig. 2 is an optical image of the final structure of example 1 of the present invention.
Fig. 3 is an optical image of the final structure of example 2 of the present invention.
Detailed Description
The invention will be further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1
(1) Preparation of PVA solution: adding 0.25g of PVA into a clean container, adding 10ml of deionized water, placing the container on a magnetic heating table, heating and stirring at 90 ℃ until the PVA is completely dissolved, and sealing, preserving and standing the solution at normal temperature to obtain a PVA solution with the mass concentration of 2.5%.
(2) Preparation of PVA film: the PDMS with the size of 4 multiplied by 4mm is cut off and stuck on a clean glass slide, 2 mu L of PVA solution is sucked by a liquid-transferring gun, the PVA solution is dripped on the PDMS to form liquid drops with the diameter of about 2mm, the tip of the liquid-transferring gun is used for scraping the PVA liquid drops to uniformly wet the PDMS, then the glass slide is placed on a heating table, the glass slide is heated at the temperature of 60 ℃ for 5 minutes, and finally, a transparent and uniform PVA film with the thickness of about 2mm is formed on the PDMS after the moisture is evaporated to dryness.
(3) Building a two-dimensional layered material heterostructure: and sequentially carrying out three ultrasonic cleaning on the silicon wafer by acetone, isopropanol and deionized water to remove impurities on the surface of the silicon wafer, and drying the surface moisture by a nitrogen gun. And repeatedly stripping a small Hexagonal Boron Nitride (HBN) sample by using an adhesive tape, adhering a sample area to a cleaned silicon wafer after the sample area is dissociated for a plurality of times, and finding a target HBN thin layer to be transferred by using a microscope. And fixing the silicon wafer with the target sample on a transfer table, inversely fixing the slide glass attached with PDMS/PVA on a mechanical arm of the transfer table, and enabling one side of the PVA film to face the silicon wafer. Operating a microscope of a transfer table to focus the thin HBN layer to be transferred on a silicon wafer, and controlling a mechanical arm to move horizontally so that the PVA film completely covers the HBN; and controlling the mechanical arm to move in the vertical direction, and attaching the glass slide to the silicon wafer, so that the PVA film and the HBN are completely attached. And fixing the mechanical arm of the transfer table, opening the heating table to heat up to 75 ℃, maintaining for 20 seconds, and stopping heating. After the silicon wafer is cooled to below 40 ℃, the PVA film is solidified, the mechanical arm is lifted, and at the moment, the HBN thin layer can be stuck by the PVA film and lifted along with the glass slide.
The replacement material is vanadium diselenide, the silicon wafer is sequentially subjected to three ultrasonic cleaning processes of acetone, polypropylene alcohol and deionized water to remove impurities on the surface of the silicon wafer, and a nitrogen gun is used for drying surface moisture. Repeatedly peeling a small sample of vanadium diselenide by using an adhesive tape, and dissociatingAfter a plurality of times, the sample area is stuck on the cleaned silicon wafer, and the silicon wafer on the transfer platform is replaced by a wafer with VSe 2 Is a silicon wafer. And (3) operating the center of the microscope of the transfer table to focus the microscope to the HBN sample level, adjusting a screw in the horizontal direction of the mechanical arm, and focusing the center of the microscope image surface to the target HBN sample. Operating the transfer stage microscope to focus the microscope on the substrate, adjusting the screw in the horizontal direction of the transfer stage to focus the center of the microscope image on the substrate VSe 2 On the sample. In the process of descending the mechanical arm, the overlapping positions of the two samples are required to be continuously adjusted until the PVA film and the silicon wafer are tightly attached. The heating table is opened, the temperature is raised to 90 ℃ for 10 seconds, the mechanical arm is slowly lifted, the PVA film can be separated from the PDMS film, and the PVA film is left on the silicon wafer.
(4) Putting the silicon wafer with the sample and the PVA film into deionized water, heating to 80 ℃, completely dissolving the PVA film after 30 minutes, taking out the substrate, lightly blowing off the surface moisture by using a helium gun, and finally obtaining the HBN coated VSe on the metal-plated silicon wafer as shown in figure 2 2 And (3) a sample.
From the optical image of FIG. 2 we can see VSe coated with thin layer HBN on a silicon substrate 2 The sample, the PVA is dissolved in water, the surface of the sample and the silicon wafer is clean enough, and the appearance of the sample is excellent.
It should be noted that, in embodiment 1 only includes a simple bilayer structure with HBN as a protective layer on a silicon wafer, in some alternative embodiments of the present invention, the whole structure step (3) may be repeated multiple times to stack different materials, and the final target substrate may have many choices.
Example 2
(1) Preparation of PVA solution: adding 0.25g of PVA into a clean container, adding 10ml of deionized water, placing the container on a magnetic heating table, heating and stirring at 90 ℃ until the PVA is completely dissolved, and sealing, preserving and standing the solution at normal temperature to obtain a PVA solution with the mass concentration of 2.5%.
(2) Preparation of PVA film: the PDMS with the size of 4 multiplied by 4mm is cut off and stuck on a clean glass slide, 2 mu L of PVA solution is sucked by a liquid-transferring gun and is dripped on a PDMS film, PVA liquid drops are scraped by the tip of the liquid-transferring gun to uniformly wet the PDMS, then the glass slide is placed on a heating table, the temperature of 60 ℃ is heated for at least 5 minutes, and after moisture is evaporated, the PVA film with the thickness of micron level and the diameter of about 2mm and transparent and uniform is finally formed on the PDMS.
(3) Building a homogeneous structure with torsion angles: and sequentially carrying out three ultrasonic cleaning on the silicon wafer by acetone, isopropanol and deionized water to remove impurities on the surface of the silicon wafer, and drying the surface moisture by a nitrogen gun. Repeatedly dissociating a small hexagonal boron nitride sample by using an adhesive tape, sticking a sample area on the cleaned silicon wafer after dissociating for a plurality of times, tearing, and finding a strip-shaped HBN thin layer to be transferred on the silicon wafer by using a microscope. And fixing the silicon wafer with the target sample on a transfer table, inversely fixing the slide glass attached with PDMS/PVA on a mechanical arm of the transfer table, and enabling one side of the PVA film to face the silicon wafer. And (3) focusing the thin HBN layer to be transferred on the silicon wafer by a microscope of the operation transfer table, and controlling the mechanical arm to move horizontally so that the PVA film completely covers the HBN.
The operation mechanical arm descends, half of the HBN and the PVA film are attached, half of the HBN and the PVA film are separated, the heating table is started to heat to 80 ℃, the Z-axis height of the mechanical arm is required to be adjusted in a fine adjustment mode continuously in the heating process, and the contact surface of the PVA film and the HBN is maintained to be free from deviation. After the temperature is maintained for 10 seconds, the mechanical arm is slightly lifted, so that the HBN sheet can be cracked along the contact surface, and if a sample cannot be torn, the temperature can be increased for multiple attempts. After splitting the sample, adjusting the angle fine adjustment screw of the mechanical arm of the transfer table to fine adjust by 0.1 degrees, adjusting the horizontal direction screw of the mechanical arm to translate and align the two HBNs to re-attach and construct the torsion angle homojunction, and lowering the mechanical arm to enable the two samples to be tightly attached. And fixing the mechanical arm of the transfer table, opening the heating table to heat up to 75 ℃, maintaining for 20 seconds, and stopping heating. After the silicon wafer is cooled to below 40 ℃, the PVA film is solidified, the mechanical arm is lifted, at the moment, the HBN homojunction can be stuck by the PVA film, and the HBN homojunction is lifted along with the glass slide.
And replacing the silicon wafer substrate plated with metal, fixing the substrate on a transfer table, operating the center of a microscope of the transfer table to focus the substrate on a sample level, adjusting a screw in the horizontal direction of a mechanical arm, and focusing the center of a microscope image surface on a target sample. The microscope of the transfer table is operated to focus the microscope on the substrate, and the horizontal direction screw of the transfer table is adjusted to focus the center of the image surface of the microscope to the target position to be transferred. Adjusting a Z-axis screw of the mechanical arm to descend the mechanical arm, enabling the boron nitride homojunction and the PVA film to be completely attached to the metal-plated silicon substrate, opening a heating table, heating to 90 ℃ and maintaining for 10s, slowly ascending the mechanical arm, enabling the PVA film to be separated from the PDMS film, and remaining on the silicon wafer.
(4) And (3) putting the silicon wafer with the sample and the PVA film into deionized water, heating to 80 ℃, completely dissolving the PVA film after 30 minutes, removing the substrate, lightly blowing off surface moisture by using a helium gun, and finally obtaining the HBN torsion angle homojunction on the silicon substrate plated with the metal.
From the optical image of fig. 3, we can see that on the silicon substrate plated with titanium-nickel metal, the twist angle homojunction sample of HBN, the final surface morphology of the substrate and the sample are excellent, and PVA has no residual trace.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (2)
1. A method for constructing a multilayer two-dimensional layered material based on a PVA film is characterized by comprising the following steps:
step 1: preparation of PVA solution:
a. adding 88000 molecular weight PVA particles into a clean container, adding a proper amount of purified water, and controlling the final solution concentration to be 2% -5%;
b. placing the container on a magnetic heating table, heating and stirring until PVA is completely dissolved, and sealing, preserving and standing the solution at normal temperature, wherein the solution is transparent and has no bubbles;
step 2: preparation of PVA film:
cutting a piece of PDMS film to be attached to a clean glass slide, sucking PVA solution by using a liquid-transferring gun, dripping the PVA solution on the PDMS film, scraping PVA liquid drops by using the tip of the liquid-transferring gun to uniformly wet the PDMS, placing the glass slide on a heating table, heating at 60 ℃ for at least 5 minutes, evaporating water to dryness, and finally forming a transparent and uniform PVA film with the thickness of micron level on the PDMS film;
step 3: building a two-dimensional layered material heterostructure:
a. sequentially carrying out three ultrasonic cleaning on a silicon wafer by acetone, isopropanol and deionized water to remove impurities on the surface of the silicon wafer, and blow-drying surface moisture by a nitrogen gun;
b. repeatedly stripping the preferred parent material by using an adhesive tape, attaching the parent material to a cleaned silicon wafer, and finding a target layered material I to be transferred by using a microscope;
c. fixing the silicon wafer processed in the step 3b on a transfer table, inversely fixing the glass slide obtained in the step 2 on a mechanical arm of the transfer table, and enabling one side of the PVA film to face the silicon wafer; operating a microscope of a transfer table to focus the target layered material I to be transferred on a silicon wafer, and controlling a mechanical arm to move horizontally so that the PVA film completely covers the target layered material I; controlling the mechanical arm to move in the vertical direction, and attaching the glass slide to the silicon wafer to enable the PVA film to be completely attached to the target layered material I;
d. fixing a mechanical arm of the transfer table, opening a heating table to heat to 75 ℃, and stopping heating after maintaining for 20 seconds; after the silicon wafer is cooled to below 40 ℃, the PVA film is solidified, the mechanical arm is lifted, the target sample I is stuck by the PVA film, and the target sample I is lifted along with the glass slide;
e. replacing a parent material, repeatedly dissociating by using an adhesive tape, attaching the parent material to a silicon wafer subjected to three ultrasonic cleaning processes of acetone, isopropanol and deionized water, finding a target layered material II to be transferred by a microscope, and replacing the silicon wafer on a transfer platform with the silicon wafer with the target layered material II; operating a transfer table microscope to focus the transfer table microscope on a target layered material II to be transferred, controlling a mechanical arm to move so that two samples are aligned to designed positions, and lowering the mechanical arm to tightly attach a glass slide and a silicon wafer to form a two-dimensional heterostructure; opening the heating table to raise the temperature to 75 ℃, and stopping heating after maintaining for 20 s; after the silicon wafer is cooled to below 40 ℃ and the PVA film is solidified, the mechanical arm is lifted, and the two-dimensional heterostructure is lifted;
step 4: transferring the two-dimensional heterostructure onto a target substrate:
a. on the basis of the step 3e, the replacement target substrate is fixed on a transfer table, a mechanical arm of the transfer table is controlled to descend, the two-dimensional heterostructure is aligned to the target substrate in the descending process, and a glass slide is tightly attached to the substrate; opening a heating table, heating to 90 ℃ for 20s, slowly lifting the mechanical arm, and leaving the PVA film on the target substrate after the PVA film is separated from the PDMS film;
b. and (3) placing the substrate with the two-dimensional heterostructure and the PVA film into purified water, heating to 80 ℃, completely dissolving the PVA film after 30 minutes, removing the substrate, lightly blowing off surface moisture by using a helium gun, and building the two-dimensional layered material heterostructure.
2. The method for constructing a multi-layered two-dimensional layered material based on a PVA film according to claim 1, wherein the step 3 may be repeated a plurality of times to stack the same or different materials, thereby forming a multi-layered two-dimensional heterostructure.
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