CN113529013B - Method for cleaving two-dimensional material by using metal adhesive tape - Google Patents

Method for cleaving two-dimensional material by using metal adhesive tape Download PDF

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CN113529013B
CN113529013B CN202110683098.5A CN202110683098A CN113529013B CN 113529013 B CN113529013 B CN 113529013B CN 202110683098 A CN202110683098 A CN 202110683098A CN 113529013 B CN113529013 B CN 113529013B
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metal
adhesive tape
layer
polymer film
metal foil
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CN113529013A (en
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罗铭砚
郭帅斐
朱瑞敏
张远波
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Fudan University
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Fudan University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005—Separation of the coating from the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

Abstract

The invention discloses a method for cleaving a two-dimensional material by using a metal adhesive tape. The metal adhesive tape comprises a polymer film layer and a metal layer; the metal layer is a metal foil layer or a metal film layer, one surface of the metal layer is tightly attached to the polymer film layer, and the other surface of the metal layer is used for contacting with a crystal material to be cleaved; the method comprises the following specific steps: placing the crystal material to be cleaved between two metal adhesive tapes, pressing with force, uncovering to make the crystal material to be cleaved adhere to the metal layer respectively, and repeating the steps for multiple times to realize the stripping of the two-dimensional material; and (3) attaching the metal adhesive tape covering the crystals to a clean substrate, then lifting the adhesive tape, and leaving the thin-layer crystals on the substrate to finish the cleavage of the two-dimensional material. The invention can solve the problem of glue residue in the prior art, obtain the two-dimensional material with clean surface, and is beneficial to preparing the heterojunction sample with clean interface and high quality in the follow-up process; the two-dimensional material obtained after cleavage has no static electricity, and the dust absorption capacity of the material can be greatly reduced.

Description

Method for cleaving two-dimensional material by using metal adhesive tape
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a method for cleaving a two-dimensional material by using a metal adhesive tape.
Background
The mechanical cleavage technology has become one of the important methods for preparing high-quality two-dimensional materials, and has shown unique advantages in the aspect of research on the intrinsic physical properties of the two-dimensional materials. The currently used mechanical cleaving method generally uses a conventional adhesive tape as a cleaving tool, i.e. a polymer film is coated with an organic glue, and the crystal material is cleaved by the adhesion of the organic glue.
The traditional mechanical cleavage method often has glue residue on the crystal material obtained after cleavage, and the material after cleavage is charged with static electricity due to the inevitable frictional electrification in the crystal replication and cleavage processes, and is easy to adsorb dust. The high-quality heterojunction sample needs the clean surface of the two-dimensional material, so that the glue residue and easy dust absorption are not beneficial to the preparation of high-quality devices, and the performance of the devices is greatly reduced.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a method for mechanically cleaving a two-dimensional material. The method utilizes the polymer film to support the metal adhesive tape to replace the traditional adhesive tape, utilizes the adhesion of metal to crystal materials to realize the cleavage of the materials, can solve the problems of adhesive residue and static electricity in the prior art, and can more efficiently obtain cleaner and higher-quality two-dimensional materials so as to prepare devices with higher performance.
In the present invention, a polymer film is used as a support, a metal is attached to the polymer film to form a tape for mechanical cleavage, and the tape is cleaved by a procedure similar to that for cleavage by a conventional tape. The crystal material to be cleaved is pressed between the two metal adhesive tapes, because the crystal is sticky with the metal, after the metal adhesive tapes are uncovered, the crystal is divided into two parts, the crystal is copied, the crystal becomes thinner gradually after the crystal is copied for multiple times, the covering area of the crystal becomes larger gradually, then the adhesive tape covering the thin crystal is pasted on a clean substrate, and then the adhesive tape is uncovered, so that the cleavage of the two-dimensional material is completed. The technical scheme of the invention is specifically introduced as follows.
A method for cleaving a two-dimensional material using a metal tape, the metal tape comprising a polymer film layer and a metal layer; the metal layer is a metal foil layer or a metal film layer, the upper surface and the lower surface of the metal layer are named as an A surface and a B surface respectively, the A surface of the metal layer is tightly attached to the polymer film layer, and the B surface is used for contacting with a crystal material to be cleaved; the method comprises the following specific steps:
step one, placing a crystal material to be cleaved between two metal adhesive tapes, pressing the two metal adhesive tapes with force, then uncovering the metal adhesive tapes to enable the crystal material to be cleaved to be adhered to the surface B of the metal layer, and repeating the step for multiple times to realize the stripping of the two-dimensional material;
and step two, attaching one surface of the metal adhesive tape covered with the thin crystal material to a clean substrate, then lifting the metal adhesive tape, dissociating the crystal, and leaving the freshly dissociated thin crystal on the substrate to finish the cleavage of the two-dimensional material.
Preferably, when the metal layer is a metal foil layer, the preparation method of the metal tape is as follows:
s1: performing surface activation treatment on the polymer film to expose dangling bonds on the surface of the polymer film;
s2: scraping an oxide layer on the upper surface of the metal foil by using a sharp object;
s3: after the polymer film with the activated surface in the step S1 is tightly attached to the upper surface of the metal foil, the polymer film and the metal foil are tightly pressed together by a tablet machine;
s4: cleaning and deoxidizing the lower surface of the metal foil at room temperature in an air atmosphere;
s5: and (5) sealing the metal foil adhesive tape treated in the step (S4) in isopropanol, transferring the metal foil adhesive tape into a glove box, and drying the metal foil adhesive tape by using inert atmosphere to finish the preparation of the metal adhesive tape.
In the step S1, the polymer film is made of a flexible polymer material, and the polymer film is made of polyimide and plays a supporting role; the surface of the polymer film is treated with oxygen plasma.
In the step S2, the metal foil is generally a metal or an alloy with relatively good ductility, the thickness of the metal foil is between 30 μm and 200 μm, the metal foil is made of a simple metal or an alloy, including but not limited to indium or gold, or indium-gallium-tin alloy, and the sharp object is a scraper, etc. The sharp object is adopted to treat the upper surface, so that the surface roughness is large, and the polymer with thermoplasticity can be attached more tightly. And fresh unoxidized indium can be exposed, the viscosity of indium and polyimide is stronger than that of indium oxide, so that the polymer film can be attached to metal more tightly by exposing fresh indium, and the metal cannot fall off in subsequent experiments.
In the step S4, firstly, soaking in acetone for 40-80S to remove organic matters on the lower surface of the metal foil, and then naturally drying on a clean bench; soaking the mixture for 40-80 s with dilute hydrochloric acid, and then sequentially soaking the mixture into deionized water and isopropanol; the cleaning and deoxidation step facilitates obtaining a clean and flat surface, which is beneficial to the subsequent crystal dissociation effect.
Preferably, when the metal layer is a metal film layer, the preparation method of the metal tape is as follows:
(1) Preparing a metal film on a substrate by using an electron beam evaporation method, a thermal evaporation method and a magnetron sputtering method;
(2) Spin-coating a polymer solution on the surface of the gold film, and then baking on a hot table to volatilize the solvent, thereby forming a polymer film on the surface of the metal film;
(3) The transparent adhesive tape is adhered to the polymer film and then peeled off, and at the same time, the metal film is peeled off, thus forming the metal adhesive tape with the exposed surface being a flat metal film with the roughness similar to that of the silicon chip.
In the step (1), the substrate is a silicon wafer, the components of the metal film are Au, pt can be used as various inert metals of the film, and the thickness of the metal film is 50-200 nm; in the step (2), the polymer is selected from any one of polymethyl methacrylate or polysiloxane. Preferably, in the step one, the crystal material to be cleaved is MoS 2 、TaS 2 、VSe 2 、FeSe、WSe 2 、WS 2 、WTe 2 BP or FeI 3 A crystalline material.
Preferably, in the step one, the metal adhesive tape and the crystal material are pressed by force, so that the crystal material to be cleaved and the metal adhesive tape are tightly attached.
Preferably, in the second step, the substrate is a silicon wafer or sapphire.
Compared with the prior art, compared with the mechanical cleavage method proposed previously, the metal foil replaces the organic glue on the traditional adhesive tape, and has the following advantages:
(1) The problem of glue residue can be solved, and the two-dimensional material with clean surface can be obtained. The two-dimensional material cleaved by the traditional adhesive tape can leave residual glue on the surface of the two-dimensional material and a substrate, and when a two-dimensional material heterojunction sample is prepared, the residual glue can be left on the interface of the two-dimensional material, so that the interface is not clean, and the mobility of the sample is reduced. Avoiding glue residues is therefore the most important advantage.
(2) The two-dimensional material after cleavage has no static electricity, and the dust absorption capacity of the material can be greatly reduced, so that the performance of a device with higher quality can be obtained.
(3) The metal adhesive tape can be used in an ultrahigh vacuum environment, and the traditional adhesive tape can be deflated in the ultrahigh vacuum environment, so that the ultrahigh vacuum is not favorably maintained.
Drawings
FIG. 1 is a schematic representation of a polymer film.
FIG. 2 is a schematic diagram showing that the oxide layer is scraped off from the surface of the metal foil by a sharp object, and the oxide layer is removed from the surface A by a sharp object.
Fig. 3. The metal foil is attached to the polymer film.
FIG. 4, removing the oxide layer on the B side of the metal foil in the metal adhesive tape.
Fig. 5. The crystal to be cleaved is placed between two metal foil tapes.
Fig. 6. The foil tape is lifted.
FIG. 7 is a drawing showing the crystalline material adhered to the tape and removed after it has been adhered to the substrate.
FIG. 8 two-dimensional MoS of example 1 with few layers cleaved on silicon wafer with example indium foil tape 2 Optical micrographs of the materials.
FIG. 9 FeI of different thicknesses cleaved on sapphire substrate with indium foil tape in example 1 3 Optical micrographs of crystalline materials.
Fig. 10 optical micrographs of black phosphorus crystalline material of different thicknesses cleaved on silicon wafers with indium foil tape in example 1.
Fig. 11 optical micrograph of black phosphorus sample cleaved on metal tape in example 2.
Reference numbers in the figures: 1-polymer film, 2-metal foil, 3-dilute hydrochloric acid solution, 4-crystal to be cleaved, and 5-substrate material.
Detailed Description
The technical scheme of the invention is explained in detail in the following by combining the drawings and the embodiment.
Example 1
The invention provides a method for cleaving a two-dimensional material by using a metal foil, which comprises the following specific steps:
s1: carrying out surface activation treatment on the polymer film (figure 1) to expose dangling bonds on the surface of the polymer; the polymer film is used as a support material, and a flexible polymer material such as polyimide is used. The support material needs to be relatively sticky to the metal foil, so that the metal foil cannot fall off the support to influence subsequent experiments in the subsequent crystal copying and cleavage processes. The polyimide is found to be more adhesive with the metal film after the plasma activation treatment, and can better support crystals in the subsequent cleavage process, so the polyimide is selected as the support.
S2, respectively naming the upper surface and the lower surface of the metal foil as an A surface and a B surface, and scraping an oxide layer on the A surface of the metal foil by using a sharp object (figure 2); the advantage of using a doctor blade to treat the oxide layer is that the roughness of the obtained A surface is large, and the A surface is tightly attached to the thermoplastic polymer; the exposed indium which is not oxidized can ensure that the polymer film and the metal film are more tightly attached; the operation of scraping the oxide layer by the scraper is simpler and more convenient than the operation of removing the oxide layer by soaking in hydrochloric acid.
S3, tightly attaching the surface-activated polymer film in the step S1 to the surface A of the metal foil, and tightly pressing the polymer film and the surface A of the metal foil together by using a tablet press to obtain a metal adhesive tape (figure 3);
s4, cleaning and deoxidizing the surface B of the metal foil in the metal foil adhesive tape at room temperature in an air atmosphere (figure 4); specifically, soaking in acetone for 40-80 s to remove organic matter on the surface B of the metal foil, and naturally drying on a clean bench; soaking the mixture for 40-80 s with dilute hydrochloric acid, and then sequentially soaking the mixture into deionized water and isopropanol; the treated B surface of the metal foil has the characteristics of cleanness and smoothness
S5: sealing the metal foil adhesive tape treated in the step S4 in isopropanol, transferring the metal foil adhesive tape into a glove box, and drying the metal foil adhesive tape by using inert atmosphere to finish the preparation of the metal foil adhesive tape;
s6: placing the crystal material to be cleaved between the metal adhesive tapes prepared in the two steps S5 (figure 5), pressing by force, and then uncovering (figure 6) to enable the crystal material to be cleaved to be respectively adhered to the two metal foil adhesive tapes; repeating the step for multiple times, continuously copying the crystal material to be cleaved, and continuously thinning the two-dimensional material on the adhesive tape;
s7, tightly attaching the master tape to a substrate (including but not limited to a silicon wafer or sapphire), and then putting the master tape into contact with the substrateUncovering (fig. 7), few layers of two-dimensional crystalline material (TaS) 2 、VSe 2 、FeSe、WSe 2 、WS 2 、WTe 2 、BP、FeI 3 Etc.) remains on the substrate.
In a specific embodiment, the metal foil is indium foil, and the polymer film is polyimide film; scraping the oxide layer on the surface A of the indium foil by a scraper; soaking in acetone for 1min to remove organic matter on the surface B of the indium foil, naturally air-drying on a clean bench, soaking in dilute hydrochloric acid for 1min, sequentially soaking in deionized water and isopropanol to remove oxidation on the surface B of the indium foil, and blow-drying in a glove box with argon; the crystal material to be cleaved adopts MoS 2 When the two adhesive tapes are used for copying the crystal, after the crystal is pasted between the two adhesive tapes, the adhesive tapes and the crystal are compressed as far as possible, and the crystal is heated for about 10 minutes at 50-80 ℃ so that the crystal to be cleaved and the metal foil are tightly attached, after the crystal and the metal foil are tightly attached, the two metal adhesive tapes are uncovered, the two-dimensional material is divided into two parts and is pasted on the two adhesive tapes, and the two-dimensional material is copied. Repeating the crystal copying step to increase the crystal covering area on the metal and thin the crystal, then attaching the adhesive tape covered with the crystal to the silicon wafer, tightly pressing the adhesive tape and the silicon wafer to make the crystal fully contact with the silicon wafer, tearing the adhesive tape, dissociating the two-dimensional material from the layers, and obtaining a single-layer or few-layer two-dimensional MoS on the substrate 2 A material. As shown in FIG. 8, the molecular structure is a MoS having a thickness of about 5nm dissociated on a silicon wafer substrate 2 And (3) sampling.
In a specific embodiment, the metal foil is indium foil, and the crystal material to be cleaved is FeI 3 The substrate is made of sapphire, and FeI with different thicknesses is obtained 3 An optical micrograph of the material is shown in fig. 9, with the thinnest sample being about 5nm.
In a specific embodiment, indium foil is used as the metal foil, black phosphorus crystals are used as the crystal material to be cleaved, silicon wafers are used as the substrate, optical micrographs of the black phosphorus materials with different thicknesses are obtained, as shown in fig. 10, and the thinnest sample is about 10 nm.
Example 2
A method for cleaving a two-dimensional material by using a metal adhesive tape comprises the following specific steps:
s1: preparing a metal film with the thickness of about 100 nm on a silicon wafer, wherein the preparation method comprises but is not limited to electron beam evaporation, thermal evaporation and magnetron sputtering;
s2: spin-coating polymer solution on the surface of the gold film, and baking on a hot table to volatilize the solvent, thereby forming a polymer film on the surface of the metal film, wherein the polymer can be polymethyl methacrylate or polysiloxane;
s3: then clinging the polymer film with a transparent adhesive tape, peeling off the transparent adhesive tape, and simultaneously peeling off the metal film to form a metal adhesive tape with a flat metal film on the exposed surface, wherein the structure of the metal adhesive tape is transparent adhesive tape/polymer film/metal film, and a layer of polymer film is added in the middle of the metal adhesive tape as a support, so that the metal film is prevented from being wrinkled, and the subsequent cleavage process is not facilitated;
s4: placing the crystal material to be cleaved between the two metal adhesive tapes prepared in the step S3, pressing the metal adhesive tapes with force, and then uncovering the metal adhesive tapes to enable the crystal material to be cleaved to be respectively adhered to the two metal adhesive tapes; repeating the step for multiple times, continuously copying the crystal material to be cleaved, and continuously thinning the two-dimensional material on the adhesive tape;
s5: and tightly attaching the adhesive tape covering the crystals to the substrate, and then removing the adhesive tape, so that a few layers of the two-dimensional crystal material are left on the substrate.
In a specific embodiment, the metal thin film is made of gold, the crystal material to be cleaved is made of black phosphorus crystal, the black phosphorus crystal is attached to the metal adhesive tape, and then the metal adhesive tape is removed, so that thin-layer crystals can be obtained on the metal adhesive tape, and optical micrographs of the black phosphorus material with different thicknesses obtained on the metal adhesive tape are shown in fig. 11, wherein the thinnest sample is about 5nm.

Claims (4)

1. A method for cleaving a two-dimensional material using a metal tape, wherein the metal tape comprises a polymer film layer and a metal layer; the metal layer is a metal foil layer or a metal film layer, the upper surface and the lower surface of the metal layer are named as an A surface and a B surface respectively, the A surface of the metal layer is tightly attached to the polymer film layer, and the B surface is used for contacting with a crystal material to be cleaved; the method comprises the following specific steps:
step one, placing a crystal material to be cleaved between two metal adhesive tapes, pressing the two metal adhesive tapes with force, then uncovering the metal adhesive tapes to enable the crystal material to be cleaved to be respectively adhered to the surfaces B of the metal layers of the two metal adhesive tapes, and repeating the step for multiple times to realize the stripping of the two-dimensional material;
step two, the surface B of the metal layer of the metal adhesive tape covering the thin crystal material is attached to a clean substrate, then the metal adhesive tape is lifted, and a few layers of two-dimensional crystal materials are left on the substrate, so that the cleavage of the two-dimensional materials is completed; wherein:
when the metal layer is a metal foil layer, the preparation method of the metal adhesive tape comprises the following steps:
s1: performing surface activation treatment on the polymer film to expose dangling bonds on the surface of the polymer film;
s2: scraping an oxide layer on the upper surface of the metal foil by using a sharp object;
s3: after the polymer film with the activated surface in the step S1 is tightly attached to the upper surface of the metal foil, the polymer film and the metal foil are tightly pressed together by a tablet machine;
s4: cleaning and deoxidizing the lower surface of the metal foil at room temperature in an air atmosphere;
s5: sealing the metal foil adhesive tape treated in the step S4 in isopropanol, transferring the metal foil adhesive tape into a glove box, and drying the metal foil adhesive tape by using inert atmosphere to finish the preparation of the metal adhesive tape; wherein:
in the step S1, polyimide is adopted as the polymer film; treating the surface of the polymer film by oxygen plasma;
in the step S2, the thickness of the metal foil is between 30 and 200 mu m, and the metal foil is made of gold, indium or indium-gallium-tin alloy material;
step S4, firstly soaking the metal foil in acetone for 40-80S, removing organic matters on the lower surface of the metal foil, and then naturally drying the metal foil on a clean bench; soaking the mixture for 40-80 s with dilute hydrochloric acid, and then sequentially soaking the mixture into deionized water and isopropanol;
when the metal layer is a metal film layer, the preparation method of the metal adhesive tape comprises the following steps:
(1) Preparing a metal film on a substrate by a thermal evaporation method or a magnetron sputtering method;
(2) Spin-coating a polymer solution on the surface of the gold film, and then baking on a hot table to volatilize the solvent, thereby forming a polymer film on the surface of the metal film;
(3) The transparent adhesive tape is tightly attached to the polymer film, the polymer film is taken off, and meanwhile, the metal film is taken off, so that the metal adhesive tape with the flat metal film on the exposed surface is formed; wherein:
in the step (1), the substrate is a silicon wafer, and the metal film comprises Au or Pt; the thickness of the metal film is between 50 nm and 200 nm;
in the step (2), the polymer is selected from any one of polymethyl methacrylate or polysiloxane.
2. The method of claim 1, wherein in step one, the crystalline material to be cleaved is MoS 2 、TaS 2 、VSe 2 、FeSe、WSe 2 、WS 2 、WTe 2 BP or FeI 3 A crystalline material.
3. The method of claim 1, wherein in the first step, the crystalline material to be cleaved and the metal tape are pressed together by force to make them fit tightly.
4. The method of claim 1, wherein in step two, the substrate is a silicon wafer or sapphire.
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