CN115650295A - Transfer method of thin-layer two-dimensional material - Google Patents

Transfer method of thin-layer two-dimensional material Download PDF

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Publication number
CN115650295A
CN115650295A CN202211190612.2A CN202211190612A CN115650295A CN 115650295 A CN115650295 A CN 115650295A CN 202211190612 A CN202211190612 A CN 202211190612A CN 115650295 A CN115650295 A CN 115650295A
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film
thin
transfer film
dimensional material
transfer
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CN202211190612.2A
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Inventor
王佩剑
洪煜堃
郑智元
潘宝俊
张致翔
蓝善贵
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ZJU Hangzhou Global Scientific and Technological Innovation Center
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ZJU Hangzhou Global Scientific and Technological Innovation Center
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Priority to CN202211190612.2A priority Critical patent/CN115650295A/en
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Abstract

The invention relates to the field of thin layer material integration and application, in particular to a transfer method of a thin layer two-dimensional material. And performing wet spin coating on the prepared thin-layer two-dimensional material to form a first transfer film, attaching a second transfer film on the first transfer film, and performing accurate transfer of the thin-layer two-dimensional material to a target substrate, an electrode or other thin-layer materials by using a micro-lens lower positioning transfer method. The invention can ensure that the material with high bonding force with the substrate can also be accurately transferred to the target position of the target substrate, realize the preparation of rare or difficult-to-grow heterojunction or accurate construction devices, and simultaneously realize the transfer application of the target substrate of ultrathin silicon and an arrayed electrode.

Description

Transfer method of thin two-dimensional material
Technical Field
The invention relates to the field of thin layer material integration and application, in particular to a transfer method of a thin layer two-dimensional material.
Background
The trend in semiconductor material and device applications is towards miniaturization, which is a strong trend towards thin, two-dimensional materials with a single atomic layer. At present, the thin two-dimensional material is a hot spot of the international material world. The two-dimensional material has special properties such as atomic-scale thickness, various component compositions, layer number dependence of properties, and the like. At present, two methods of transferring two-dimensional materials mainly include dry transfer and wet transfer. Dry transfer is transfer by using adhesive film adhesive material; after the wet transfer is to spin coat the high polymer, the original substrate is etched off, and then the target substrate is used to fish the medium film and transfer the medium film to the target substrate. However, both of them have advantages and disadvantages, for example, dry transfer can achieve precise transfer but is only suitable for mechanically peeled materials with weak bonding force to the substrate, while those two-dimensional materials synthesized by chemical vapor deposition method or the like at high temperature have strong bonding force to the substrate, and dry transfer is not suitable. While the wet transfer can transfer the material with strong bonding force with the substrate, it cannot realize the precise transfer of the two-dimensional material with micro-scale, and the precise positioning transfer of the material is necessary for the subsequent device fabrication, integration and application.
Disclosure of Invention
The invention provides a transfer method of a thin two-dimensional material, which overcomes the defects of the prior art and comprises the following steps:
providing an initial substrate, wherein a thin two-dimensional material layer is formed on the surface of the initial substrate;
forming a first transfer film on the surfaces of the initial substrate and the thin two-dimensional material, wherein the contact surface of the first transfer film and the thin two-dimensional material is a first surface, the opposite surface of the first surface is a second surface, and the adhesion force of the first transfer film and the thin two-dimensional material is greater than that of the initial substrate and the thin two-dimensional material;
peeling a thin layer of two-dimensional material from the initial substrate surface with the first transfer film;
adhering a second transfer film on the second surface of the first transfer film, and positioning and transferring the thin two-dimensional material and the first transfer film to the surface of the target substrate by using the second transfer film;
and sequentially removing the second transfer film and the first transfer film to realize the transfer of the thin two-dimensional material to the target substrate.
Optionally, the second transfer film is a thermal release transfer adhesive film.
Optionally, the heat release transfer adhesive film is a PDMS adhesive film, a PBS adhesive film, or a PVC adhesive film.
Optionally, the method for removing the second transfer film comprises: heating to 80-100 deg.C to release heat from the second transfer film.
Optionally, the first transfer film is one of a PS film, a PMMA film, a PVA film, a PC film, and a PCL film.
Optionally, when the first transfer film is a PS film, the process for forming the PS film includes: and spin-coating a PS toluene solution on the surfaces of the initial substrate and the thin-layer two-dimensional material, firstly performing spin-coating at the rotating speed of 500rpm for 15 seconds and the acceleration of 100-150rpm/s, then performing spin-coating at 3000rpm for 60 seconds and the acceleration of 400-500rpm/s, and then heating to 100 ℃ for baking and keeping for 60 seconds to form a PS film.
Optionally, the PS toluene solution is a PS solution prepared by adding 150-175mg of polystyrene into 1ml of toluene solution.
Optionally, the method for removing the first transfer film comprises: the target substrate to which the PS film is adhered is immersed in toluene to remove the PS film.
Optionally, before the second transfer film is adhered to the surface of the first transfer film, a slit is formed at an edge of the first transfer film, a small amount of deionized water is injected, the first transfer film and the thin two-dimensional material adhered to the surface of the first transfer film are peeled from the initial substrate, and the peeled second surface of the first transfer film is adhered to the second transfer film.
Optionally, the thin two-dimensional material is one of molybdenum disulfide, tungsten disulfide, graphene, tungsten diselenide, platinum selenide, boron nitride, indium selenide, ultrathin silicon, and arrayed electrodes.
In conclusion, the invention has the beneficial effects that:
the embodiment of the invention provides a transfer method of a thin-layer two-dimensional material, which comprises the steps of spin-coating a first transfer film on the surface of the prepared thin-layer two-dimensional material, and then effectively and accurately transferring the specific thin-layer two-dimensional material to a target substrate, an electrode or the thin-layer two-dimensional material by a positioning transfer method under a microscope. The transfer method of the thin-layer two-dimensional material provided by the invention can change wet transfer into accurate transfer, can accurately transfer the thin-layer two-dimensional material with high bonding force with the substrate to the target position of the target substrate, and is beneficial to realizing the preparation of rare or difficult-to-grow heterojunction or accurate construction devices.
Drawings
FIG. 1 is a schematic illustration of steps of a method of transferring a thin two-dimensional layer of material according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an initial substrate having a thin two-dimensional material layer for a method of transferring a thin two-dimensional material layer according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a thin two-dimensional material transfer method according to an embodiment of the present invention after spin-coating a first transfer film;
fig. 4 is a schematic diagram illustrating a bonding structure between a second surface of a first transfer film and a second transfer film in the thin two-dimensional material transfer method according to the embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a thin two-dimensional material after being peeled from an initial substrate according to an embodiment of the present invention;
fig. 6 is a schematic structural diagram illustrating a second transfer film and target substrate bonding step of the thin two-dimensional material transfer method according to the embodiment of the present invention;
fig. 7 is a schematic structural view illustrating a step of separating the first transfer film from the second transfer film and adhering the first transfer film to the target substrate in the transfer method of the thin two-dimensional material according to the embodiment of the present invention;
fig. 8 is a schematic structural diagram of a transfer method of a thin two-dimensional material according to an embodiment of the present invention after removing the first transfer film.
Detailed Description
The present invention will be described in further detail below with reference to specific examples in order to facilitate understanding by those skilled in the art.
An embodiment of the present invention provides a method for transferring a thin two-dimensional material, please refer to fig. 1, which includes:
s100, providing an initial substrate 10, wherein a thin two-dimensional material 20 is formed on the surface of the initial substrate 10;
s200, forming a first transfer film 30 on the surfaces of the initial substrate 10 and the thin two-dimensional material 20, wherein the contact surface of the first transfer film 30 and the thin two-dimensional material 20 is a first surface, the opposite surface of the first surface is a second surface, and the adhesion force of the first surface of the first transfer film 30 and the thin two-dimensional material 20 is greater than that of the initial substrate 10 and the thin two-dimensional material 20;
s300, peeling off a thin two-dimensional material 20 from the surface of the initial substrate 10 by using the first transfer film 30;
s400, adhering a second transfer film 40 on the second surface of the first transfer film 30, and positioning and transferring the thin two-dimensional material 20 and the first transfer film 30 to the surface of the target substrate 60 by using the second transfer film 40;
and S500, sequentially removing the second transfer film 40 and the first transfer film 30 to realize the transfer of the thin two-dimensional material 20 to the target substrate 60.
Specifically, step S100 is performed to provide an initial substrate 10, and a thin two-dimensional material 20 is formed on a surface of the initial substrate 10.
In the embodiment of the present invention, referring to fig. 2, the thin two-dimensional material 20 is a thin two-dimensional material 20 insoluble in a toluene solution.
In the embodiment of the present invention, the thin two-dimensional material 20 is one of molybdenum disulfide, tungsten disulfide, graphene, tungsten diselenide, platinum selenide, boron nitride, indium selenide, ultra-thin silicon, and an arrayed electrode. In other embodiments, the thin layer of two-dimensional material may be other two-dimensional materials.
In the embodiment of the present invention, the initial substrate 10 is a graphite substrate, and the thin two-dimensional material 20 is formed on the surface of the initial substrate 10 by a deposition process, including but not limited to chemical vapor deposition. In other embodiments, the initial substrate may also be a silicon substrate, a sapphire substrate, or the like.
Step S200 is executed to form a first transfer film 30 on the surface of the initial substrate 10 and the thin two-dimensional material 20, wherein the contact surface of the first transfer film 30 and the thin two-dimensional material 20 is a first surface, the opposite surface of the first surface is a second surface, and the adhesion force of the first transfer film 30 and the thin two-dimensional material 20 is greater than the adhesion force of the initial substrate 10 and the thin two-dimensional material 20.
The first transfer film 30 is one of a PS (Polystyrene) film, a PMMA (Polymethyl methacrylate) film, a PVA (polyvinyl alcohol) film, a PC (Polycarbonate) film, and a PCL (Polycaprolactone) film.
In the embodiment of the present invention, referring to fig. 3, when the first transfer film 30 is a PS film, the process steps for forming the PS film are as follows: and spin-coating a PS toluene solution on the surfaces of the initial substrate 10 and the thin two-dimensional material 20, firstly performing spin-coating at the rotation speed of 500rpm for 15 seconds and the acceleration of 100-150rpm/s, then performing spin-coating at 3000rpm for 60 seconds and the acceleration of 400-500rpm/s, and then heating to 100 ℃ for baking and keeping for 60 seconds to form a PS film.
In the embodiment of the invention, the PS toluene solution is prepared by adding 150-175mg of polystyrene into 1ml of toluene solution, and the preparation steps specifically comprise: taking 300-350mg of polystyrene, and adding 2ml of toluene solution into the polystyrene to prepare a mixed solution; and heating the mixed solution to 50-60 ℃, and simultaneously carrying out accelerated dissolution on the mixed solution by utilizing ultrasound to prepare the PS solution.
The surface of the two-dimensional material is coated with a PS film in a spin mode, and the PS film is baked, so that the PS film and the two-dimensional material are better bonded together, and the two-dimensional material can be simultaneously peeled from the initial substrate 10 when the PS film is peeled.
Step S300 is performed to peel off the thin two-dimensional material 20 from the surface of the initial substrate 10 by using the first transfer film 30.
In an embodiment of the present invention, referring to fig. 4, a gap is formed at the edge of the first transfer film 30, a small amount of deionized water is injected to peel the first transfer film 30 and the thin two-dimensional material 20 adhered to the surface of the first transfer film 30 from the initial substrate 10.
In the embodiment of the present invention, the breach of the edge of the first transfer film 30 is formed by etching the starting substrate 10, so that the first transfer film 30 at the breach formation position is less adhesive to the starting substrate 10.
In the embodiment of the present invention, the process of peeling the first transfer film 30 from the initial substrate 10 is wet transfer.
The wet transfer enables the thin two-dimensional material with high bonding force with the initial substrate to be stripped from the initial substrate with high success rate, and the stripping effect is excellent.
Step S400 is executed, please refer to fig. 4, the second surface of the first transfer film 30 is attached to the surface of the second transfer film 40, and the thin two-dimensional material 20 and the first transfer film 30 are positioned and transferred to the surface of the target substrate 60 by using the second transfer film 40.
In the embodiment of the present invention, the second transfer film 40 is used to adhere the first transfer film 30 having the thin two-dimensional material 20 on the surface detached from the original substrate 10.
In an embodiment of the present invention, referring to fig. 5, the thin two-dimensional material 20 is tightly combined with the first transfer film 30, and the first transfer film 30 is tightly combined with the second transfer film 40, so as to facilitate the transfer of the thin two-dimensional material 20.
In an embodiment of the present invention, the second transfer film 40 is a thermal release transfer film, and the thermal release transfer film is a PDMS (Polydimethylsiloxane) film, a PBS (Polybutylene succinate) film, or a PVC (Polyvinyl chloride) film.
In the embodiment of the present invention, the second transfer film 40 is a PDMS adhesive film, which has optical total transparency, so as to facilitate accurate positioning of a microscope of a transfer platform, and the PDMS adhesive film has a property of being easily bonded to the first transfer film 30 at a normal temperature, so that the second transfer film 40 and the first transfer film 30 are better bonded; the heat release of the PDMS adhesive film in a heated state makes it easy to separate from the first transfer film 30.
In the embodiment of the present invention, referring to fig. 6, a first surface of the first transfer film 30 faces the target substrate 60, and a second surface of the first transfer film 30 faces the microscope of the transfer stage.
The target substrate 60 is a silicon substrate, electrode or other thin layer material. In an embodiment of the invention, the target substrate surface has an electrode 50, and the target substrate 60 serves as a basis for the construction of devices and heterojunctions.
In other embodiments, the target substrate surface may not have an electrode.
In the embodiment of the invention, the electrode 50 is used as a bottom electrode of a device, and a thin two-dimensional material layer is formed on the surface of the electrode 50 to prepare a corresponding semiconductor device.
In the embodiment of the present invention, referring to fig. 7, the specific steps of transferring the thin two-dimensional material 20 are as follows: firstly, a target substrate 60 is placed on the surface of a two-dimensional material transfer platform, the position of the target substrate 60 to be accurately transferred is found through a microscope 70 of the transfer platform, a second transfer film 40 attached with a first transfer film 30 is adhered to a glass slide, a thin two-dimensional material 20 to be accurately transferred is found on the first transfer film 30 through the microscope 70 of the transfer platform, and the first transfer film 30 and the second transfer film 40 with the thin two-dimensional material 20 are pressed downwards until the target substrate 60 is attached.
Step S500 is executed to sequentially remove the second transfer film 40 and the first transfer film 30, and to transfer the thin two-dimensional material 20 to the target substrate 60.
In the embodiment of the present invention, the method for removing the second transfer film 40 includes: and heating the second transfer film 40 to 80-100 ℃, continuously heating the second transfer film 40 for 5 minutes, and lifting off the second transfer film 40 after the preset time is reached to realize the heat release of the first transfer film 30 from the second transfer film 40.
The heated second transfer film 40 is easily separated from the first transfer film 30, and the first transfer film 30, the thin two-dimensional material 20 and the target substrate 60 are more closely attached by the heat treatment.
In an embodiment of the present invention, referring to fig. 8, the method for removing the first transfer film 30 includes: the target substrate 60 to which the PS film is adhered is immersed in toluene to remove the PS film.
In the embodiment of the present invention, when the first transfer film 30 is a PS film, the target substrate 60 to which the PS film is adhered is immersed in toluene for a period of time of 3 to 24 hours to remove the PS film.
In other embodiments, the solution to remove the first transfer membrane is other suitable solutions.
In the embodiment of the present invention, the target substrate 60 with the PS film removed is taken out of the toluene, the thin two-dimensional material 20 is adhered to the target substrate 60, the target substrate 60 with the thin two-dimensional material 20 adhered thereto is washed with a small amount of toluene, the target substrate 60 with the thin two-dimensional material 20 adhered thereto is washed with deionized water, and finally the target substrate 60 with the thin two-dimensional material 20 adhered thereto is dried by a nitrogen gun, and the whole transfer process is completed.
Finally, it is to be noted that any modifications or equivalent substitutions of some or all of the technical features made by the method of the present invention and the technical solutions of the examples described above may be made without departing from the corresponding technical solutions of the present invention, and the obtained essence belongs to the method of the present invention and the patent scope of the embodiments described above.

Claims (10)

1. A method for transferring a thin two-dimensional layer of material, comprising:
providing an initial substrate, wherein a thin two-dimensional material layer is formed on the surface of the initial substrate;
forming a first transfer film on the surfaces of the initial substrate and the thin two-dimensional material, wherein the contact surface of the first transfer film and the thin two-dimensional material is a first surface, the opposite surface of the first surface is a second surface, and the adhesion force of the first transfer film and the thin two-dimensional material is greater than that of the initial substrate and the thin two-dimensional material;
peeling the thin layer of two-dimensional material from the initial substrate surface with the first transfer film;
pasting a second transfer film on the second surface of the first transfer film, and positioning and transferring the thin two-dimensional material and the first transfer film to the surface of a target substrate by using the second transfer film;
and sequentially removing the second transfer film and the first transfer film to realize the transfer of the thin two-dimensional material to the target substrate.
2. A method of transferring a laminar two-dimensional material according to claim 1, wherein the second transfer film is a thermal release transfer film.
3. The method of claim 2, wherein the thermal release transfer adhesive film is a PDMS adhesive film, a PBS adhesive film or a PVC adhesive film.
4. A method of transferring a thin two-dimensional material as claimed in claim 2, wherein the second transfer film is removed by: heating to 80-100 ℃ to achieve heat release of the first transfer film from the second transfer film.
5. A method of transferring a thin two-dimensional material as claimed in claim 1, wherein said first transfer film is one of PS film, PMMA film, PVA film, PC film, PCL film.
6. The method of claim 1, wherein when the first transfer film is a PS film, the process steps for forming the PS film are: and spin-coating a PS toluene solution on the surfaces of the initial substrate and the thin-layer two-dimensional material, firstly performing spin-coating at the rotation speed of 500rpm for 15 seconds and at the acceleration of 100-150rpm/s, then performing spin-coating at the rotation speed of 3000rpm for 60 seconds and at the acceleration of 400-500rpm/s, heating to 100 ℃, baking and keeping for 60 seconds to form a PS film.
7. The method of claim 6, wherein the PS toluene solution is a PS solution prepared by adding 150-175mg of polystyrene to 1ml of toluene solution.
8. A method of transferring a thin layer of two-dimensional material as defined in claim 7, wherein the method of removing the first transfer film comprises: and immersing the target substrate adhered with the PS film into toluene to remove the PS film.
9. A method as claimed in claim 1, wherein before the second transfer film is adhered to the surface of the first transfer film, a slit is formed at the edge of the first transfer film, a small amount of deionized water is injected to peel the first transfer film and the thin two-dimensional material adhered to the surface of the first transfer film from the initial substrate, and the peeled second surface of the first transfer film is adhered to the second transfer film.
10. The method of claim 1, wherein the thin two-dimensional material is one of molybdenum disulfide, tungsten disulfide, graphene, tungsten diselenide, platinum selenide, boron nitride, indium selenide, ultra-thin silicon, and arrayed electrodes.
CN202211190612.2A 2022-09-28 2022-09-28 Transfer method of thin-layer two-dimensional material Pending CN115650295A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107170711A (en) * 2017-04-26 2017-09-15 中山大学 It is a kind of to shift the method for preparing two-dimensional atomic crystal laminated construction
CN110676218A (en) * 2019-08-28 2020-01-10 西安工业大学 Method for preparing two-dimensional transition metal sulfide by directional transfer CVD (chemical vapor deposition) method
CN111704128A (en) * 2020-05-27 2020-09-25 东南大学 Two-dimensional material transfer method based on substrate with steps
CN111874896A (en) * 2020-06-17 2020-11-03 中国科学院合肥物质科学研究院 Method for accurately transferring two-dimensional material and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107170711A (en) * 2017-04-26 2017-09-15 中山大学 It is a kind of to shift the method for preparing two-dimensional atomic crystal laminated construction
CN110676218A (en) * 2019-08-28 2020-01-10 西安工业大学 Method for preparing two-dimensional transition metal sulfide by directional transfer CVD (chemical vapor deposition) method
CN111704128A (en) * 2020-05-27 2020-09-25 东南大学 Two-dimensional material transfer method based on substrate with steps
CN111874896A (en) * 2020-06-17 2020-11-03 中国科学院合肥物质科学研究院 Method for accurately transferring two-dimensional material and application thereof

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