CN116190211B - Method for transferring two-dimensional material based on nano microcavity structure substrate - Google Patents
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Abstract
The invention discloses a method for transferring a two-dimensional material based on a substrate with a nano microcavity structure, and belongs to the technical field of two-dimensional material transfer. The method specifically comprises the following steps: firstly, preparing a PDMS/glass slide structure; transferring the two-dimensional material to the surface of the PDMS by using a mechanical stripping method, and shearing off redundant PDMS films; then preparing a target substrate with a nano microcavity structure by utilizing a nano imprinting technology and a plasma etching technology; finally, the two-dimensional material is successfully attached to the target substrate under the guidance of the operation principle of slow release and fast lifting by controlling the speed of the transfer platform. The transfer of the two-dimensional material by the method can reduce the residual glue on the surface of the two-dimensional material and the bubbles at the interface, so that the uniform and clean high-quality two-dimensional material is obtained, the two-dimensional material is not damaged in the preparation process, the combination of the two-dimensional material and the micro-nano structure material is efficiently realized, and the application prospect of the two-dimensional material can be effectively widened.
Description
Technical Field
The invention relates to the technical field of two-dimensional material transfer, in particular to a method for transferring two-dimensional materials based on a substrate with a nanometer microcavity structure.
Background
The two-dimensional material is a material with electrons capable of freely moving only on nano-scale (1-100 nm) in two dimensions, such as a nano film, a superlattice, a quantum well and the like, and currently commonly used two-dimensional materials include graphene, molybdenum disulfide, tungsten disulfide, boron nitride and the like.
After the first discovery of graphene in 2004, two-dimensional materials have been widely focused on due to their unique physical and chemical properties, and have shown very broad application prospects in the fields of biological detection, microelectronics, and the like. Compared with silicon-based materials, two-dimensional materials have atomic-level thickness and surface dangling bond-free properties, and have little short channel effect, so that the two-dimensional materials are expected to be used in next-generation integrated circuits. Since the two-dimensional material is bonded to the target substrate primarily by van der Waals forces, it can be bonded to any substrate in theoryOn the bottom, the use scene of the two-dimensional material is greatly expanded. However, most two-dimensional materials are grown in Cu, ni, pt, au, si, siO 2 On substrate materials, in order to realize the representation, application and device preparation of the two-dimensional material, the two-dimensional material is often required to be transferred from an initial substrate material to various target matrixes such as quartz, silicon chips and PET, and in order to be capable of carrying out effective transfer, the development of a perfect and efficient two-dimensional material transfer technology is particularly important.
The combination of the two-dimensional material and the micro-nano structure material has important research significance in the field of optical engineering, but the substrate is not smooth enough, and the interface cleanliness is difficult to reach the standard, so that the method faces great challenges in the actual preparation process. The two-dimensional material transfer method which is common at present mainly comprises two main types of wet transfer and dry transfer.
Among them, wet transfer mainly includes a substrate etching method and an electrochemical bubbling method. The main flow of the substrate etching method is as follows: spin-coating a PMMA film on the surface of a two-dimensional material grown on a metal substrate by using a spin coater, heating to solidify the PMMA film, then placing the PMMA film into an etching solution to etch the metal substrate, taking PMMA as a transfer medium to protect the two-dimensional material at the moment, finally drying, placing a two-dimensional material/PMMA composite on a target substrate, and cleaning the PMMA film by using acetone to remove the PMMA film, thereby completing the transfer step. The disadvantage of the substrate etching method is that the metal ion contamination of the etching solution and PMMA residues on the surface of the two-dimensional material transferred by the method can not be completely removed, and the metal ion contamination and polymer particles of tens to hundreds of nanometers can seriously affect the optical and electrical properties of the two-dimensional material and the performance of devices. The electrochemical bubbling method comprises the following specific steps: firstly, PMMA is spin-coated on the surface of graphene/copper foil, then the graphene/copper foil is placed in an electrolytic cell to serve as a cathode, external voltage is applied, small current is applied, separation of the PMMA/graphene and the copper foil is achieved by utilizing a large amount of hydrogen bubbles generated by Cu surface water decomposition, and after washing and drying, the PMMA is removed by washing with acetone, so that graphene transfer is completed. The electrochemical bubbling method has high efficiency, but has the problem of PMMA residue, and has high and uncontrollable speed of the electrochemical bubbling process, and is easy to break two-dimensional materials, so that the mechanical strength of a transfer medium/two-dimensional material system is required to be certain.
Dry transfer includes several methods, roll-to-roll, mechanical lift-off, PDMS assisted transfer. Although these methods can also achieve transfer of two-dimensional materials, each also has some problems, in particular: the two-dimensional material transferred by roll to roll is poor in quality, and a large amount of impurities remain on the surface and a rigid substrate cannot be used; the mechanical stripping transfer method has strong randomness, and is easy to cause material waste; the PDMS stripping transfer method is simple and easy to use by using a viscoelastic PDMS polymer film as a carrier to transfer the two-dimensional material, but the adhesion force is weak when the PDMS is used for mechanically stripping the two-dimensional material, the stripping process is difficult, and the surface of the transferred two-dimensional material still has the problems of PDMS residues, wrinkles, bubbles and the like, so that the method is also unfavorable for preparing devices based on high-quality two-dimensional materials, and the performance of the devices is greatly reduced. However, it is worth mentioning that the advantages of the PDMS assisted transfer method are also obvious, the method has no high polymer spin coating and the whole process does not contact any solution, thus providing possibility for the transfer of the two-dimensional material which is easy to hydrolyze and absorb moisture; and no special requirement is made on the substrate because no more foreign impurities are introduced. Therefore, it is very important to further optimize the PMDS (Polydimethylsiloxane) assisted transfer method, so that the technology of transferring the two-dimensional material with clean interface on the micro-nano structure surface can be realized. However, it should be noted that when the target substrate has a micro-nano structure, the adsorption capability of the substrate to the material is correspondingly reduced, and the success rate of dry transfer may be reduced.
In order to solve the above problems, a series of targeted researches have been conducted by those skilled in the art, for example, a method for transferring a two-dimensional material onto a hole substrate is disclosed in chinese patent CN 113851371A, which adjusts the viscosity of a PDMS film by changing the temperature, so as to successfully transfer the two-dimensional material onto a silicon substrate with holes, and in order to increase the success rate, the lifting rate of the PDMS film after contacting with the material is also purposely reduced. However, although this method realizes the combination of two-dimensional material and hole substrate compared with the conventional PDMS stripping transfer method, it has certain disadvantages, and particularly shows that: 1. the PDMS is heated at high temperature, so that a layer of glue is remained on the surface of the two-dimensional material, and the performance of the two-dimensional material is affected; 2. it is not suitable for the transfer of thin layer two-dimensional materials; 3. the method is a redesign of a transfer scheme aiming at a substrate with a hole structure, and is mainly used for successfully transferring a two-dimensional material to the substrate with the hole, but the interface adhesion after the transfer cannot be guaranteed to be tight, no air bubbles, wrinkles and other bad conditions exist, that is, the transfer quality of the two-dimensional material cannot be guaranteed; 4. in general, when the two-dimensional material is transferred onto a planar substrate, the adsorption force is larger when the peeling speed of the PDMS film is high, and the two-dimensional material is adsorbed on the surface of the PDMS polymer film; on the contrary, when the peeling speed is low, the adsorption force is smaller, and the two-dimensional material is more prone to be adsorbed on the surface of the target substrate, so that the transfer process is usually completed by adopting a method of 'fast slow start', and the transfer success rate is improved by adopting a method of 'slow start', however, the fact that when the target substrate is provided with the micro-nano cavity structure is clear is that the actual contact area between the two-dimensional material and the substrate is smaller, and the 'slow start' can enable a part of the junction between the two-dimensional material and the substrate not to be contacted with the micro-nano structure substrate, so that the phenomenon that the two-dimensional material can fall on the surface of the substrate completely is difficult, and folds, bubbles and the like can occur at the junction.
Therefore, in order to achieve efficient and high quality transfer of two-dimensional materials on micro-nanostructure substrates, further exploration and improvement of the transfer process is still needed.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for transferring a two-dimensional material based on a substrate with a nano microcavity structure, which can solve the problems of impurity residues, material wrinkles, interface bubbles and the like in the existing transfer method, obtain a two-dimensional material with a clean surface and is beneficial to preparing a heterojunction sample with a clean interface and high quality subsequently.
In order to achieve the technical purpose, the invention is realized by the following technical scheme: a method for transferring two-dimensional materials based on a substrate with a nanometer microcavity structure comprises the following steps:
1) Attaching a PDMS film to a glass slide to obtain a PDMS/glass slide structure;
2) Transferring the two-dimensional material to be transferred onto the PDMS film by using a mechanical stripping method to form a glass slide/PDMS/two-dimensional material structure, and cutting off the redundant PDMS film by taking the two-dimensional material to be transferred as the center;
3) Preparing a seal, and transferring a nano array structure on the seal to a photoresist coating layer on a substrate material through a nano imprinting technology;
4) Carrying out plasma etching treatment on the substrate material coated with the photoresist to obtain a target substrate with a nano microcavity structure;
5) Fixing a glass slide with materials in a substrate clamping groove of a transfer table, and placing a target substrate on a sample seat of the transfer table;
6) And the two-dimensional material is attached to the surface of the target substrate after being separated from the PDMS by controlling the attaching and separating speed of the transfer platform.
Further, in the step 2), the two-dimensional material is graphene, boron nitride or molybdenum disulfide.
Further, UV-O is used before transferring the two-dimensional material to the PDMS film 3 And (3) treating the surface of the PDMS film.
Further, the two-dimensional material transferred to the PDMS film was uniform, wrinkle-free, and 0.3-70 a nm a thick.
Further, in the step 4), the prepared target substrate with the nano microcavity structure has the microcavity diameter of 570-710nm.
Further, in step 6), when the two-dimensional material is transferred, the slide glass should be slowly put down first to make the two-dimensional material adhere to the target substrate, the adhering time is 3-5min (the adhering time is mainly based on the area of the two-dimensional material, the area is large, the adhering time is long), the slide glass needs to be continuously lowered by 10 μm at a speed of 0.5 μm/s after adhering, and the slide glass needs to be quickly lifted at a speed of 180-210 μm/s after maintaining for 2min, so that the two-dimensional material is completely transferred to the surface of the target substrate.
The transfer of the two-dimensional material is performed according to the principle of 'slow release and fast lifting', because 'slow release' can reduce wrinkles generated by strain of the two-dimensional material, and secondly, the slow transfer speed can uniformly attach the two-dimensional material to the surface of the substrate, so that bubbles at an interface are reduced. The air bubbles are lowered for a certain height after bonding, mainly for discharging the air bubbles at the joint, so that the air bubbles can be further diffused into the microcavity; the two-dimensional material and the substrate can be further tightly attached by maintaining the attaching state for 2 min; the principle of atmospheric pressure is mainly applied in the process of quick-lifting after bonding, because the surface area of the array microcavity structure distributed on the whole target substrate is about 1/4 of the surface area of the whole substrate, the cavity structure has a large proportion, if the bonding is slow-lifting, a part of the bonding boundary line between the two-dimensional material and the microcavity substrate is not contacted with the target substrate, the contact surface is small, and the two-dimensional material is difficult to fall on the surface of the target substrate; the method is characterized in that the two-dimensional material is not adsorbed, the boundary line is not generated at a time of quick start, the two-dimensional material is separated from the two-dimensional material rapidly, the two-dimensional material is dropped on the surface of the microcavity substrate, the two-dimensional material is uniformly stressed around the microcavity substrate because the slow start always moves in one direction, and meanwhile, the stress is not uniform because the hole exists, so that the left side of the hole is always lifted up, then the hole is equivalent to contact with the atmosphere, and a part of the hole belongs to a suspension state and is not contacted with the microcavity substrate, so that no acting force exists, the two-dimensional material cannot adsorb, the two-dimensional material is easily combined with the substrate because the two-dimensional material is quickly separated, the two-dimensional material is quickly dropped on the surface of the microcavity substrate, and the two-dimensional material is uniformly stressed around the microcavity substrate because the two-dimensional material is required to be thin when the two-dimensional material is required to be separated, and the two-dimensional material is more easily combined with the substrate because the two-dimensional material is required to be separated when the two-dimensional material is thin.
The beneficial effects of the invention are as follows:
1. according to the method, the microcavity with uniform rank is prepared on the substrate material by utilizing the nanoimprint technology and the plasma etching technology, and due to the existence of the microcavity, bubbles can be further diffused into the microcavity in the two-dimensional material transferring process, so that the two-dimensional material after transferring is tightly attached to the target substrate without bubbles;
2. the method and the device follow the operation principle of slow release and fast lifting to transfer the two-dimensional material, the slow release process can reduce bubbles and wrinkles at the interface, the fast lifting process mainly utilizes the atmospheric pressure principle, and the two-dimensional material and the target substrate can be more tightly attached together by utilizing the resistance existing in the lifting process, so that the combination of the two-dimensional material and the micro-nano structure material is successfully realized;
3. according to the method, after the two-dimensional material is uniformly attached to the surface of the substrate, the glass slide is required to be continuously lowered by a certain height, and the operation is mainly to enable bubbles generated in the attaching process of the two-dimensional material and the substrate to be further extruded and diffused into the microcavity, so that the transferred two-dimensional material is smooth and free of bubbles, and the quality of the transferred two-dimensional material is effectively improved;
4. the transfer platform is used for transferring the two-dimensional material, the two-dimensional material can be precisely transferred to any position of the target substrate, the stress in the transfer process is uniform, and no new wrinkles are generated;
5. the present application utilizes UV-O 3 The PDMS film is pretreated, so that the viscosity of the PDMS film is weakened, the adsorption of impurities on the surface of the material is reduced, and the residual glue on the surface of the transferred two-dimensional material can be greatly reduced after the two-dimensional material is successfully transferred;
6. the method disclosed by the application has universality and can be used for successfully transferring two-dimensional materials such as grapheme, transition metal chalcogenide, boron nitride and the like with different thicknesses.
Drawings
FIG. 1 is an SEM image of a micro-nano structured substrate prepared according to example one;
FIG. 2 is a flow chart of the preparation of a micro-nanostructure substrate;
FIG. 3 is an optical microscope image at 100 Xmagnification of the two-dimensional boron nitride material transferred in example 1;
FIG. 4 is an Atomic Force Microscope (AFM) image of the two-dimensional boron nitride material transferred in example 1;
FIG. 5 is thickness test data for the two-dimensional boron nitride material transferred in example 1;
FIG. 6 is an optical microscope image at 100 Xmagnification of the transferred two-dimensional graphene material in example 2;
FIG. 7 is an Atomic Force Microscope (AFM) image of the two-dimensional graphene material transferred in example 2;
FIG. 8 is thickness test data for the two-dimensional graphene material transferred in example 2;
FIG. 9 is an optical microscope image at 100 Xmagnification of the transferred two-dimensional molybdenum disulfide material in example 3;
FIG. 10 is an Atomic Force Microscope (AFM) image of the two-dimensional molybdenum disulfide material transferred in example 3;
fig. 11 is thickness test data for the two-dimensional molybdenum disulfide material transferred in example 3.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the present invention without departing from the spirit of the invention are intended to be within the scope of the present invention.
Example 1 method of transferring two-dimensional boron nitride Material based on micro-nanostructure substrate
Step 1) preparing a seal at room temperature: mixing SIP (Pt) 1 drop, VDT (3.4 g) and SIT (2 drops), stirring with clean glass rod for 2min to thoroughly mix, adding HMS (1 g), and stirring again for 2min for use;
after the mould is purged by a nitrogen gun, the mould is placed in a culture dish, the prepared mixed solution is poured on the surface of the mould, the mould is opened by the nitrogen gun, the surface of the mould is uniformly covered with the mixed solution, and the mould is placed in a drying box at 75 ℃ for 10 min.
Step 2) mixing and stirring the curing agent and PDMS according to the volume ratio of 1:10, pouring the mixture into the sample treated in the step 1, and carrying out vacuumizing treatment to overflow bubbles due to the fact that air enters during stirring; and after the bubbles overflow completely, placing the mixture into a 75 ℃ drying box for treatment for 20 min, and obtaining the seal with the nano array structure.
Step 3) spin-coating photoresist SU8 with the mass concentration of 4 percent on a silicon wafer (spin-coating rotating speed of 3000 r/min, acceleration of 500 r/s and spin-coating time length of 30 s), processing for 1 min at a heating table (65 ℃) after spin-coating is finished, processing for 1 min at the heating table (95 ℃), cooling at room temperature, pressing a structure on a seal on the silicon wafer spin-coated with SU8, and pressing for 35 seconds at the temperature of 95 ℃.
Step 4) placing the sample in RIE equipment, transferring the nano array structure on the initial seal onto photoresist on a silicon wafer by utilizing a nano imprinting technology, and etching the sample by using an RIE-150 reactive ion etching instrument to remove redundant photoresist on the surface of the silicon wafer: first at O 2 Etching part of the photoresist under the conditions of 50 sccm strength, 30 w power, 100 high valve and 30S etching time to expose the silicon wafer substrate; reuse of CBrF 3 And SF (sulfur hexafluoride) 6 The mixture of gases (gas flow ratio 100/10 sccm, power 100W, high valve 100) etches 140S to further etch the exposed silicon layer to an etch depth of 55 nm; finally use O 2 The photoresist was removed by gas (stationary instrument power 30 w, O 2 The flow rate was 50 sccm, and the treatment time 240 s). As shown in fig. 1, the surface of the silicon-based substrate after treatment is provided with microcavity structures distributed in an array, the diameter of a single cavity is 600 nm, and the cavity depth is 55 nm. (the preparation flow of the nano microcavity structure is shown in FIG. 2).
Step 5) shearing PDMS into small blocks with the length of 0.5 cm x 2 cm, removing the film on the surface of the small blocks, and attaching the small blocks to a glass slide, wherein the UV-O film is formed by 3 Treating PDMS surface, repeatedly adhering blue film/two-dimensional material, transferring BN on the blue film onto PDMS, finding out small-layer uniform non-wrinkled BN under microscope, cutting PDMS film into blocks of 0.3 cm by 0.3 cm (cutting off redundant film, and separating boundary of material from film)The boundary needs to be reserved with a certain width, so that the two-dimensional material is positioned in the center of the sheared film as much as possible, and the later transfer is facilitated).
Step 6) on a transfer platform (the function of the transfer platform is to find a target sample and align with a substrate to be transferred, a glass slide with a material is fixed in a substrate clamping groove of the transfer platform, a silicon-based substrate is adsorbed on a sample seat of the transfer platform, the transfer platform can slowly lift and enable a two-dimensional material to be slowly attached to the surface of the substrate), the transfer platform is slowly lowered to completely attach the two-dimensional material to the substrate by using a slow-release and fast-lifting method, the attaching process needs to last for about 3 min, and the transfer platform is continuously lowered for 10 mu m at a rate of 0.5 mu m/s; after relaxation for 2min, the boron nitride is rapidly separated at a speed of 200 mu m/s, the transferred boron nitride is observed under an optical microscope (figure 3), no residual glue and bubbles are observed, and after the transferred boron nitride is photographed by an Atomic Force Microscope (AFM) (figure 4), the method is proved to be capable of transferring to obtain a high-quality two-dimensional material.
Example 2 method of transferring two-dimensional graphene Material based on micro-nanostructure substrate
The present example differs from example 1 only in that the two-dimensional graphene material was transferred in this example, the corresponding steps and process parameters were the same as in example 1, the transferred graphene was observed under an optical microscope (fig. 6), no residual glue, wrinkles and bubbles were found, and the transferred graphene was photographed with an Atomic Force Microscope (AFM) (fig. 7), again confirming that a high quality two-dimensional material could be transferred using the present method.
Example 3 method for transferring two-dimensional molybdenum disulfide Material based on micro-nano Structure substrate
This example differs from example 1 only in that the two-dimensional molybdenum disulfide material was transferred in this example, and the corresponding steps and process parameters were the same as those in example 1, and the transferred molybdenum disulfide was observed under an optical microscope (fig. 9), without residual glue, wrinkles and bubbles, and the transferred molybdenum disulfide was photographed by an Atomic Force Microscope (AFM) (fig. 10), and it was also confirmed that a high-quality two-dimensional material could be transferred by the present method.
The foregoing has outlined and described the basic principles, features, and advantages of the present invention. However, the foregoing is merely specific examples of the present invention, and the technical features of the present invention are not limited thereto, and any other embodiments that are derived by those skilled in the art without departing from the technical solution of the present invention are included in the scope of the present invention.
Claims (5)
1. The method for transferring the two-dimensional material based on the substrate with the nano microcavity structure is characterized by comprising the following steps of:
1) Attaching a PDMS film to a glass slide to obtain a PDMS/glass slide structure;
2) Transferring the two-dimensional material to be transferred onto the PDMS film by using a mechanical stripping method to form a glass slide/PDMS/two-dimensional material structure, and cutting off the redundant PDMS film by taking the two-dimensional material to be transferred as the center;
3) Preparing a seal, and transferring a nano array structure on the seal to a photoresist coating layer on a substrate material through a nano imprinting technology;
4) Carrying out plasma etching treatment on the substrate material coated with the photoresist to obtain a target substrate with a nano microcavity structure;
5) Fixing a glass slide with materials in a substrate clamping groove of a transfer table, and placing a target substrate on a sample seat of the transfer table;
6) The two-dimensional material is attached to the surface of the target substrate after being separated from the PDMS by controlling the attaching and separating speed of the transfer platform;
in the step 6), when the two-dimensional material is transferred, the glass slide is firstly slowly put down to enable the two-dimensional material to be attached to the target substrate, the attaching time is 3-5min, the glass slide is required to be continuously lowered by 10 mu m at the speed of 0.5 mu m/s after attaching, and the glass slide is quickly lifted at the speed of 180-210 mu m/s after maintaining for 2min, so that the two-dimensional material is completely transferred to the surface of the target substrate.
2. The method for transferring two-dimensional materials based on the substrate with the nanometer microcavity structure according to claim 1, wherein in the step 2), the two-dimensional materials are graphene, boron nitride or molybdenum disulfide.
3. The method for transferring two-dimensional material based on the substrate with the nano-microcavity structure according to claim 1, wherein UV-O is used before the two-dimensional material is transferred onto the PDMS film 3 And (3) treating the surface of the PDMS film.
4. The method for transferring two-dimensional material based on the substrate with the nanometer microcavity structure according to claim 1, wherein the two-dimensional material transferred onto the PDMS film is uniform and has no wrinkles, and the thickness is 0.3-70nm.
5. The method for transferring two-dimensional materials based on a substrate with a nano microcavity structure according to claim 1, wherein in the step 4), the diameter of the microcavity on the prepared target substrate with the nano microcavity structure is 570-710nm.
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| EP3386914A1 (en) * | 2015-12-12 | 2018-10-17 | Forschungszentrum Jülich GmbH | Method for transferring graphene pieces onto a substrate |
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| CN112694127A (en) * | 2020-12-18 | 2021-04-23 | 北京科技大学 | Method for regulating and controlling semimetal characteristics of two-dimensional transition metal chalcogenide nanosheets |
| CN113200523A (en) * | 2021-03-25 | 2021-08-03 | 华南师范大学 | Stripping and transferring method of large-area layered two-dimensional material |
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| US20170217777A1 (en) * | 2016-01-30 | 2017-08-03 | Massachusetts Institute Of Technology | Transfer Method for Two-Dimensional Film |
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| CN112694127A (en) * | 2020-12-18 | 2021-04-23 | 北京科技大学 | Method for regulating and controlling semimetal characteristics of two-dimensional transition metal chalcogenide nanosheets |
| CN113200523A (en) * | 2021-03-25 | 2021-08-03 | 华南师范大学 | Stripping and transferring method of large-area layered two-dimensional material |
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