CN113529013A - 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

Info

Publication number
CN113529013A
CN113529013A CN202110683098.5A CN202110683098A CN113529013A CN 113529013 A CN113529013 A CN 113529013A CN 202110683098 A CN202110683098 A CN 202110683098A CN 113529013 A CN113529013 A CN 113529013A
Authority
CN
China
Prior art keywords
metal
layer
adhesive tape
film
polymer film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110683098.5A
Other languages
Chinese (zh)
Other versions
CN113529013B (en
Inventor
罗铭砚
郭帅斐
朱瑞敏
张远波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fudan University
Original Assignee
Fudan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fudan University filed Critical Fudan University
Priority to CN202110683098.5A priority Critical patent/CN113529013B/en
Publication of CN113529013A publication Critical patent/CN113529013A/en
Application granted granted Critical
Publication of CN113529013B publication Critical patent/CN113529013B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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. an organic glue is coated on the polymer film, 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 the oxide layer on the upper surface of the metal foil by using a sharp object;
s3: closely attaching the surface-activated polymer film in the step S1 to the upper surface of the metal foil, and tightly pressing the polymer film and the metal foil together by a tablet press;
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 processed 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 for supporting; the surface of the polymer film is treated with oxygen plasma.
In 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. 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, the metal foil is firstly soaked in acetone for 40 to 80 seconds to remove organic matters on the lower surface of the metal foil, and then the metal foil is naturally dried 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 MoS2、TaS2、VSe2、FeSe、WSe2、WS2、WTe2BP or FeI3A crystalline material.
Preferably, in the step one, the metal tape and the crystal material are pressed by force, so that the crystal material to be cleaved and the metal 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 the 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 shows 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 the 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 tape2Optical micrographs of the materials.
Fig. 9.FeI of different thicknesses cleaved on sapphire substrate with indium foil tape in example 13Optical 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 the crystal in the subsequent cleavage process, so the polyimide is selected as the support.
S2, respectively naming the upper and lower surfaces of the metal foil as A surface and B surface, and scraping the oxide layer on the A surface of the metal foil by 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, after the polymer film with the activated surface in the step S1 is tightly attached to the surface A of the metal foil, the polymer film and the metal foil are tightly pressed together by a tablet machine 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 processed 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 two metal adhesive tapes prepared in the step S5 (fig. 5), pressing the crystal material with force, and then uncovering the crystal material (fig. 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 closely attaching the master tape to a substrate (including but not limited to silicon wafer or sapphire), and then peeling off the master tape (FIG. 7), wherein the master tape has a few layers of two-dimensional crystal material (TaS)2、VSe2、FeSe、WSe2、WS2、WTe2、BP、FeI3Etc.) 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 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 MoS2When 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. The step of crystal replication is repeated and,the covering area of the crystals on the metal is increased, the crystals become thin, the adhesive tape covered with the crystals is attached to the silicon wafer, the adhesive tape and the silicon wafer are tightly pressed to enable the crystals to be fully contacted with the silicon wafer, the adhesive tape is torn, the two-dimensional material is dissociated from the layers, and single-layer or few-layer two-dimensional MoS obtained on the substrate2A material. As shown in FIG. 8, it is a MoS dissociated to a thickness of about 5nm on a silicon wafer substrate2And (3) sampling.
In a specific embodiment, the metal foil is indium foil, and the crystal material to be cleaved is FeI3The substrate is made of sapphire, and FeI with different thicknesses is obtained3An optical micrograph of the material is shown in fig. 9, with the thinnest sample being about 5 nm.
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 on a silicon wafer, wherein the thickness of the metal film is about 100 nm, and 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 forcibly, 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, then lifting the adhesive tape, and leaving a few layers of the two-dimensional crystal material 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 crystals, a metal adhesive tape is used to adhere the black phosphorus crystals to the metal thin film, then the adhesive tape is removed, thin crystal layers can be obtained on the metal adhesive tape, optical micrographs of the black phosphorus material with different thicknesses obtained on the metal adhesive tape are shown in fig. 11, and the thinnest sample is about 5 nm.

Claims (10)

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:
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 dissociated into two halves from the layers, and respectively adhering the two halves 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;
and step two, attaching the surface B of the metal layer of the metal adhesive tape covering the thin-layer crystal material to a clean substrate, then lifting the metal adhesive tape, dissociating part of crystals from the layers again, leaving half of the crystals on the adhesive tape and the other half of the crystals on the substrate, and needing to leave the freshly dissociated thin-layer crystals on the substrate, thereby completing the cleavage of the two-dimensional material.
2. The method of claim 1, wherein when the metal layer is a metal foil layer, the metal tape is prepared by the following method:
s1: performing surface activation treatment on the polymer film to expose dangling bonds on the surface of the polymer film;
s2: scraping the oxide layer on the upper surface of the metal foil by using a sharp object;
s3: closely attaching the surface-activated polymer film in the step S1 to the upper surface of the metal foil, and tightly pressing the polymer film and the metal foil together by a tablet press;
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 processed 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.
3. The method according to claim 2, wherein in step S1, the polymer film is polyimide; the surface of the polymer film is treated with oxygen plasma.
4. The method of claim 2, wherein in step S2, the metal foil has a thickness of 30-200 μm, and is made of elemental metal indium or a metal alloy material, including gold or indium-gallium-tin alloy.
5. The method according to claim 2, wherein in step S4, the metal foil is first soaked in acetone for 40S to 80S to remove organic substances from the lower surface of the metal foil, and then naturally dried on a clean bench; soaking the mixture for 40-80 s with dilute hydrochloric acid, and then soaking the mixture into deionized water and isopropanol.
6. The method of claim 1, wherein when the metal layer is a metal film layer, the metal tape is prepared by the following steps:
(1) preparing a metal film on a substrate by an electron beam evaporation method, 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 stuck to the polymer film and then peeled off, and at the same time, the metal film is peeled off, so that the metal adhesive tape with the flat metal film on the exposed surface is formed.
7. The method according to claim 6, wherein in the step (1), the substrate is a silicon wafer, and the metal thin film is composed of a plurality of inert metals which can be formed into a thin film, including Au, 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.
8. The method of claim 1, wherein in step one, the crystalline material to be cleaved is MoS2、TaS2、VSe2、FeSe、WSe2、WS2、WTe2BP or FeI3A crystalline material.
9. 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.
10. The method of claim 1, wherein in step two, the substrate is a silicon wafer or sapphire.
CN202110683098.5A 2021-06-21 2021-06-21 Method for cleaving two-dimensional material by using metal adhesive tape Active CN113529013B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110683098.5A CN113529013B (en) 2021-06-21 2021-06-21 Method for cleaving two-dimensional material by using metal adhesive tape

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110683098.5A CN113529013B (en) 2021-06-21 2021-06-21 Method for cleaving two-dimensional material by using metal adhesive tape

Publications (2)

Publication Number Publication Date
CN113529013A true CN113529013A (en) 2021-10-22
CN113529013B CN113529013B (en) 2023-02-10

Family

ID=78125301

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110683098.5A Active CN113529013B (en) 2021-06-21 2021-06-21 Method for cleaving two-dimensional material by using metal adhesive tape

Country Status (1)

Country Link
CN (1) CN113529013B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113582125A (en) * 2021-07-21 2021-11-02 深圳清华大学研究院 Ultra-smooth packaging device and packaging method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100170626A1 (en) * 2007-05-24 2010-07-08 Basf Se Method for the production of polymer-coated metal foils, and use thereof
CN106458602A (en) * 2014-06-20 2017-02-22 加利福尼亚大学校董会 Method for fabrication and transfer of graphene
CN210765123U (en) * 2019-10-28 2020-06-16 常熟市海洲电子材料有限公司 High-temperature-resistant polyimide adhesive tape
JP2020199707A (en) * 2019-06-11 2020-12-17 Ａｐｃ株式会社 Laminate and method for manufacturing the same
CN112670160A (en) * 2020-12-22 2021-04-16 中国科学院半导体研究所 Preparation method of two-dimensional material substrate compatible with molecular beam epitaxy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100170626A1 (en) * 2007-05-24 2010-07-08 Basf Se Method for the production of polymer-coated metal foils, and use thereof
CN106458602A (en) * 2014-06-20 2017-02-22 加利福尼亚大学校董会 Method for fabrication and transfer of graphene
JP2020199707A (en) * 2019-06-11 2020-12-17 Ａｐｃ株式会社 Laminate and method for manufacturing the same
CN210765123U (en) * 2019-10-28 2020-06-16 常熟市海洲电子材料有限公司 High-temperature-resistant polyimide adhesive tape
CN112670160A (en) * 2020-12-22 2021-04-16 中国科学院半导体研究所 Preparation method of two-dimensional material substrate compatible with molecular beam epitaxy

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113582125A (en) * 2021-07-21 2021-11-02 深圳清华大学研究院 Ultra-smooth packaging device and packaging method thereof
CN113582125B (en) * 2021-07-21 2023-06-06 深圳清华大学研究院 Super-slip packaging device and packaging method thereof

Also Published As

Publication number Publication date
CN113529013B (en) 2023-02-10

Similar Documents

Publication Publication Date Title
TWI485756B (en) Thin wafer structure and method
JP4995626B2 (en) Manufacturing method of bonded substrate
CN113529013B (en) Method for cleaving two-dimensional material by using metal adhesive tape
TW200416813A (en) Method of producing SOI wafer and SOI wafer
US5753563A (en) Method of removing particles by adhesive
CN111362309B (en) Method for transferring perovskite oxide film by using soluble supporting layer
CN106289898A (en) The preparation method of the molybdenum bisuphide TEM sample that a kind of number of plies is controlled
CN106672956A (en) Large-scale graphene transferring method
CN102867740A (en) Non-destructive and pollution-free graphical method for nano-carbon film
TW201008670A (en) Cleaning apparatus and cleaning method
CN113683083B (en) Method for high-cleanliness lossless transfer of graphene nanoribbons
CN110963460B (en) Two-dimensional material cleavage method
CN104229770B (en) The method improving CNT parallel array density by elastomeric material Poisson's ratio
KR20180009450A (en) Nanofilm transfer method and apparatus
TWI645969B (en) Multilayer graphene soft board transfer method and graphene soft board group
JPH08264740A (en) Coupled wafer and production thereof
JP3534847B2 (en) Method for removing foreign matter adhering to semiconductor wafer
CN110217785B (en) Transfer operation method of CVD-grown graphene
JPH08124892A (en) Adhesive tape for removing impurity attached to semiconductor wafer and removal
CN115246657B (en) Method for transferring two-dimensional material
CN115650295A (en) Transfer method of thin-layer two-dimensional material
JP2007194345A (en) Method and device for manufacturing laminate substrate
CN110954570A (en) Method for stripping two-dimensional material grown on sapphire substrate by temperature control bubbling
US11961637B1 (en) Stretchable composite electrode and fabricating method thereof
JP2012059965A (en) Manufacturing method and manufacturing device for glued wafer

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant