CN105789549A - Method for preparing electrode on two-dimensional material - Google Patents

Abstract

A simple and controllable method for preparing electrodes on two-dimensional materials according to the present invention belongs to the field of material science and electronic technology. The polymer film (5) is fixed on the smooth surface of the adhesive tape (4), and transferred to the target position of the two-dimensional material (2) by the microscopic manipulator and pressed tightly, and the carrier net (3) and the two-dimensional material (2) Metal electrodes are deposited on the top, the grid (3) is removed with tweezers, and a microelectrode (7) is obtained on the two-dimensional material (2). The method of the invention has low requirements on equipment, mild conditions and simple operation; and the shape and size of the electrode can be conveniently adjusted only by changing the type of the carrier net, and has wide applicability.

Description

A method for preparing electrodes on two-dimensional materials

technical field

The invention belongs to the field of material science and electronic technology, and relates to a simple and controllable method for preparing electrodes on two-dimensional materials.

Background technique

Two-dimensional materials such as graphene, transition metal dichalcogenides, boron nitride, and two-dimensional polymers have attracted extensive attention from researchers due to their unique properties, and are expected to be widely used in the fields of micro batteries, supercapacitors, transistors, and microelectronic devices. widely used. Among them, the preparation of electrodes on the surface of two-dimensional materials is the key to basic scientific research and practical applications. However, the small size and various shapes of 2D materials make the preparation of microelectrodes difficult. At present, researchers mainly prepare electrodes on the surface of two-dimensional materials through microfabrication methods such as ultraviolet lithography, electron beam deposition, and focused ion beam deposition. Among them, the ultraviolet lithography method needs to go through processes such as glue coating, ultraviolet exposure, development, and etching. Not only are the steps cumbersome, but it is also easy to cause damage to the two-dimensional material. Electron beam deposition and focused ion beam deposition can deposit electrodes at specified positions on two-dimensional materials, but the required equipment is expensive, the operation is cumbersome, time-consuming, and it is easy to cause radiation damage to two-dimensional polymers, affecting performance characterization . Therefore, the field still needs to develop a simple and widely applicable method for preparing electrodes on two-dimensional materials.

Contents of the invention

The technical problem to be solved by the present invention is to overcome the problems existing in the background technology and provide a simple and controllable method for preparing electrodes on two-dimensional materials, which is used to prepare electrodes with controllable shapes and sizes at the target positions of various two-dimensional materials. The microelectrode can avoid damage and damage to the two-dimensional material during the preparation process, and has a wide range of applications, easy operation, and short time-consuming.

The specific technical scheme is as follows:

A method for preparing an electrode on a two-dimensional material, comprising the following steps:

1) Transfer the two-dimensional material 2 onto the SiO ₂ /Si substrate 1;

2) Punch a small hole with a diameter of 1 to 2.5 mm on the tape 4 with a hole puncher;

3) Stick the carrier net 3 on the adhesive surface of the adhesive tape 4, wherein the center point of the carrier net 3 coincides with the center point of the small hole on the adhesive tape 4;

4) fixing the polymer film 5 on the smooth surface of the adhesive tape 4, the thickness of the polymer film 5 being 1-5 mm;

5) The assembly of the carrier grid 3/adhesive tape 4/polymer film 5 obtained in step 4) is installed on the glass slide 6 on the microscopic manipulator and the assembly is transferred to the second step in step 1) using the microscopic manipulator. At the target position of the two-dimensional material 2, make the side of the assembly with the carrier net 3 face the two-dimensional material 2 and compress it;

6) Slowly lift the micromanipulator described in step 5) vertically, and remove the polymer film 5, and obtain a two-dimensional material 2 covering the grid 3 and the adhesive tape 4 on the SiO ₂ /Si substrate 1;

7) Depositing a metal electrode with a thickness of 50nm to 200nm on the grid 3, the adhesive tape 4 and the two-dimensional material 2;

8) Remove the grid 3 and the adhesive tape 4 with tweezers, and obtain the microelectrode 7 on the two-dimensional material 2 .

In a method for preparing an electrode on a two-dimensional material of the present invention, the two-dimensional material 2 is preferably graphene, molybdenum disulfide, tungsten disulfide, titanium dioxide, boron nitride or a two-dimensional polymer; The two-dimensional size of the dimensional material is preferably 200nm×500nm～10cm×10cm, and the thickness is preferably 0.3nm～100μm; the thickness of the SiO ₂ layer in the SiO ₂ /Si substrate 1 is preferably 100～500nm; the small The hole diameter is preferably 2 mm.

In a method for preparing an electrode on a two-dimensional material according to the present invention, the carrier grid 3 may be a copper grid, a nickel grid, a gold grid, a titanium grid or a molybdenum grid.

In a method for preparing an electrode on a two-dimensional material of the present invention, the polymer film 5 described in step 4) is fixed on the smooth surface of the adhesive tape 4, the smooth surface of the adhesive tape 4 and the polymer film 5 can be used The adhesive force between is fixed; The preferred polydimethylsiloxane film of described polymer film 5, polyethylene terephthalate film, polymethyl methacrylate film or polyvinyl chloride film; The thickness of the object film 5 is preferably 3mm.

In a method for preparing an electrode on a two-dimensional material of the present invention, step 5) can be performed under an optical microscope.

In a simple and controllable method for preparing electrodes on two-dimensional materials of the present invention, the metal electrode described in step 7) is preferably a gold electrode, a platinum electrode, a tungsten electrode or a nickel electrode; the thickness of the metal electrode is preferably 100nm; the metal electrode The shape and size of the electrodes can be adjusted by choosing different grids.

Compared with the prior art, the present invention has the following beneficial effects:

1. The method of the present invention is operated under an optical microscope, which can accurately position and deposit electrodes at designated positions of two-dimensional materials.

2. The method of the present invention can realize the preparation of electrodes by using ordinary evaporation equipment, which has low equipment requirements and is easy to operate; and only by changing the type of the carrier net, the shape and size of the electrodes can be adjusted conveniently.

3. The electrode prepared by the method of the present invention has good adhesion and small contact resistance; under the premise of ensuring better electrode quality, the operation is carried out under milder conditions, and more importantly, avoiding the use of various two-dimensional Material damage and destruction, wide applicability.

Description of drawings:

Fig. 1 is an optical microscope image of transferring a two-dimensional material onto a SiO ₂ /Si substrate in step 1) of the present invention.

Fig. 2 is a schematic diagram of an adhesive tape with a carrier net obtained in step 3) of the present invention.

Fig. 3 is a structural schematic diagram of step 4) of the present invention to fix the adhesive tape on the polymer film.

Fig. 4 is a schematic diagram of a glass slide after installing a polymer film in step 5) of the present invention.

Fig. 5 is a schematic diagram of step 5) of the present invention to transfer the polymer film with the grid and adhesive tape onto the two-dimensional material.

Fig. 6 is a schematic diagram of a two-dimensional material covered with a carrier grid and adhesive tape obtained in step 6) of the present invention.

Fig. 7 is a schematic diagram of a two-dimensional material after depositing a metal electrode in step 7) of the present invention.

Fig. 8 is a schematic diagram of the two-dimensional material of the prepared microelectrode after removing the grid in step 8) of the present invention.

FIG. 9 is an optical microscope image of the two-dimensional material after the microelectrode is prepared in Example 1.

The reference signs in the above figures are: 1 is SiO ₂ /Si substrate, 2 is two-dimensional material, 3 is grid, 4 is adhesive tape, 5 is polymer film, 6 is glass slide, 7 is microelectrode .

detailed description

The present invention will be further described below in combination with specific embodiments. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content of the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Example 1

1) Transfer two-dimensional polyporphyrin to SiO ₂ (300nm)/Si substrate (note: 300nm refers to the thickness of SiO ₂ , and the numbers in brackets in the following embodiments all indicate the thickness of SiO ₂ ), see the attached figure 1. In this embodiment, the two-dimensional material 2 is two-dimensional polyporphyrin. From the optical microscope picture in Figure 1, it can be seen that the size of the two-dimensional polyporphyrin within the field of view is about 5 μm × 50 μm, and the thickness is 4 nm;

2) Use a puncher to punch holes on the adhesive tape to obtain an adhesive tape with small holes, and the diameter of the small holes is 2mm;

3) 2000 mesh copper mesh is fixed on the sticky surface of the adhesive tape with small holes obtained in step 2), to obtain an adhesive tape with 2000 mesh copper mesh, wherein the center point of the copper mesh coincides with the center point of the small hole;

4) Fix the smooth surface of the adhesive tape with 2000-mesh copper mesh obtained in step 3) on the polydimethylsiloxane film, and the thickness of the polydimethylsiloxane film is 2mm;

5) The polydimethylsiloxane film with the copper mesh and adhesive tape obtained in step 4) is installed on the glass slide on the micromanipulator and transferred to the SiO ₂ ( 300nm)/Si substrate on the target position of the two-dimensional polyporphyrin and compacted;

6) Slowly lift the micromanipulator vertically, and remove the polydimethylsiloxane film, and obtain a two-dimensional polyporphyrin covered with copper mesh and tape on the SiO ₂ (300nm)/Si substrate;

7) Depositing a gold electrode with a thickness of 100nm on the copper mesh, adhesive tape and two-dimensional polyporphyrin;

8) After depositing the electrodes, use tweezers to remove the copper mesh and tape to obtain microelectrodes on the 2D polyporphyrin. Its optical microscope picture is as shown in Figure 9, it can be seen from the figure that the microelectrode prepared by the method of the present invention is clear and distinct, the electrode quality is high, and after the gold electrode is deposited, the two-dimensional polyporphyrin has a good morphology. It shows that the method of the present invention does not cause damage and destruction to the two-dimensional material.

Example 2

1) transfer graphene to SiO ₂ (200nm)/Si substrate;

2) Use a puncher to punch holes on the adhesive tape to obtain an adhesive tape with small holes, the diameter of which is 1.5mm;

3) 1000 mesh nickel meshes are fixed on the sticky surface of the adhesive tape with small holes obtained in step 2), to obtain tapes with 1000 mesh nickel meshes, wherein the central point of the nickel mesh coincides with the central point of the small holes;

4) the smooth surface of the adhesive tape with 1000 mesh nickel mesh obtained in step 3) is fixed on the polyethylene terephthalate film, and the thickness of the polyethylene terephthalate film is 3mm;

5) The polyethylene terephthalate film with the nickel mesh and adhesive tape obtained in step 4) was mounted on a glass slide on the micromanipulator and transferred to the SiO2 film in step 1) using the micromanipulator. ₂ (200nm)/Si substrate on the target position of graphene and compacted;

6) Slowly lift the micromanipulator vertically, remove the polyethylene terephthalate film, and obtain graphene covered with nickel mesh and adhesive tape on the SiO ₂ (200nm)/Si substrate;

7) Depositing a platinum electrode with a thickness of 150nm on nickel mesh, adhesive tape and graphene;

8) After depositing the electrode, remove the nickel mesh and tape with tweezers, and obtain a microelectrode on the graphene.

Example 3

1) transfer molybdenum disulfide to SiO ₂ (500nm)/Si substrate;

2) Use a puncher to punch holes on the adhesive tape to obtain an adhesive tape with small holes, the diameter of which is 2.5 mm;

3) Fixing the 800 mesh titanium mesh on the sticky surface of the adhesive tape with small holes obtained in step 2) to obtain an adhesive tape with 800 mesh titanium mesh, wherein the central point of the titanium mesh coincides with the central point of the small hole;

4) The smooth surface of the adhesive tape with 800 mesh titanium mesh obtained in step 3) is fixed on the polymethyl methacrylate film, and the thickness of the polymethyl methacrylate film is 4mm;

5) The polymethyl methacrylate film with the titanium mesh and adhesive tape obtained in step 4) is installed on the glass slide on the micromanipulator and transferred to the _SiO2 (500nm )/Molybdenum disulfide target position on the Si substrate and compacted;

6) Slowly lift the micromanipulator vertically, remove the polymethyl methacrylate film, and obtain molybdenum disulfide covered with titanium mesh and tape on the SiO ₂ (500nm)/Si substrate;

7) Depositing a tungsten electrode with a thickness of 50nm on the titanium mesh, adhesive tape and molybdenum disulfide;

8) After the electrodes are deposited, the titanium mesh and tape are removed with tweezers to obtain microelectrodes on molybdenum disulfide.

Example 4

1) Transfer boron nitride onto SiO ₂ (100nm)/Si substrate;

2) Use a puncher to punch holes on the adhesive tape to obtain an adhesive tape with small holes, the diameter of which is 1mm;

3) Fix the 1500-mesh gold mesh on the sticky surface of the adhesive tape with small holes obtained in step 2) to obtain an adhesive tape with 1500-mesh gold mesh, wherein the center point of the gold mesh coincides with the center point of the small hole;

4) the smooth surface of the adhesive tape with 1500 mesh gold mesh obtained in step 3) is fixed on the polyvinyl chloride film, and the thickness of the polyvinyl chloride film is 1mm;

5) The polyvinyl chloride film with the gold mesh and adhesive tape obtained in step 4) is installed on the glass slide on the micromanipulator and transferred to the SiO ₂ (100nm)/SiO2 (100nm)/Si boron nitride on the substrate at the target position and compacted;

6) Slowly lift the micromanipulator vertically, remove the polyvinyl chloride film, and obtain boron nitride covered with gold mesh on the SiO ₂ (100nm)/Si substrate;

7) Depositing a nickel electrode with a thickness of 200nm on the gold mesh, adhesive tape and boron nitride;

8) After depositing the electrodes, use tweezers to remove the gold mesh and tape, and obtain microelectrodes on boron nitride.

Example 5

1) transfer tungsten disulfide to SiO ₂ (400nm)/Si substrate;

2) Use a puncher to punch holes on the adhesive tape to obtain an adhesive tape with small holes, and the diameter of the small holes is 2mm;

3) the molybdenum mesh is fixed on the sticky surface of the adhesive tape with small holes obtained in step 2), and the adhesive tape with molybdenum mesh is obtained, wherein the central point of the molybdenum mesh coincides with the central point of the small hole;

4) The smooth surface of the adhesive tape with molybdenum mesh obtained in step 3) is fixed on the polydimethylsiloxane film, and the thickness of the polydimethylsiloxane film is 5mm;

5) The polydimethylsiloxane film with molybdenum mesh and adhesive tape obtained in step 4) is installed on the glass slide on the micromanipulator and transferred to the _SiO2 (400nm )/Si substrate on the target position of tungsten disulfide and compacted;

6) Slowly lift the micromanipulator vertically, remove the polydimethylsiloxane film, and obtain tungsten disulfide covered with molybdenum mesh on the SiO ₂ (400nm)/Si substrate;

7) Depositing a gold electrode with a thickness of 100nm on the molybdenum mesh and tungsten disulfide;

8) After the electrodes are deposited, the molybdenum mesh is removed with tweezers, and a microelectrode is obtained on the tungsten disulfide.

It should be noted that the diagrams provided by the present invention are only schematic diagrams illustrating the basic configuration of the present invention, so only the components related to the present invention are shown in the diagrams rather than the number, shape and size of the components in actual implementation Drawing, the type, quantity and proportion of each component can be changed at will during its actual implementation, and its component layout type may also be more complicated.

Claims (6)

1. the method preparing electrode in two-dimensional material, has following steps:

1) two-dimensional material (2) is transferred to SiO₂In/Si substrate (1)；

2) adopting card punch above to make a call to a diameter at adhesive tape (4) is the aperture of 1～2.5mm；

3) being bonded in the adhesive faces of adhesive tape (4) by load net (3), the central point of the central point and the aperture on adhesive tape (4) that wherein carry net (3) overlaps；

4) being fixed on the shiny surface of adhesive tape (4) by thin polymer film (5), the thickness of described thin polymer film (5) is 1～5mm；

5) by step 4) to be arranged on microtechnique microscope slide (6) on hand upper and utilize microtechnique hands that assembly is transferred to step 1 for the assembly of load net (3)/adhesive tape (4)/thin polymer film (5) that obtains) in the target location of two-dimensional material (2), make assembly and compress towards two-dimensional material (2) with the side of load net (3)；

6) by step 5) described in microtechnique hands slowly vertically pick up, and removing polymer thin film (5), at SiO₂/ Si substrate (1) obtains covering the two-dimensional material (2) of load net (3) and adhesive tape (4)；

7) in load net (3) adhesive tape (4) and two-dimensional material (2), deposit the metal electrode of 50nm～200nm thickness；

8) remove load net (3) and adhesive tape (4) with tweezers, two-dimensional material (2) obtains microelectrode (7).

2. a kind of method preparing electrode in two-dimensional material according to claim 1, it is characterised in that described two-dimensional material (2) is Graphene, molybdenum bisuphide, tungsten disulfide, titanium dioxide, boron nitride or two-dimensional polymer；The two-dimensional of described two-dimensional material is 200nm × 500nm～10cm × 10cm, and thickness is 0.3nm～100 μm；Described SiO₂SiO in/Si substrate (1)₂The thickness of layer is 100～500nm；The described hole diameter on adhesive tape (4) is 2mm.

3. a kind of method preparing electrode in two-dimensional material according to claim 1, it is characterised in that described load net (3) is copper mesh, nickel screen, gold net, titanium net or molybdenum net.

4. a kind of method preparing electrode in two-dimensional material according to claim 1, it is characterized in that, step 4) described in thin polymer film (5) is fixed on the shiny surface of adhesive tape (4), be utilize adhesion between the shiny surface of adhesive tape (4) and thin polymer film (5) fixing；Described thin polymer film (5) is polydimethylsiloxanefilm film, pet film, polymethyl methacrylate film or polyvinyl chloride film；The thickness of thin polymer film (5) is 3mm.

5. a kind of method preparing electrode in two-dimensional material according to claim 1, it is characterised in that step 5) it is operated under an optical microscope.

6. according to the arbitrary a kind of described method preparing electrode in two-dimensional material of Claims 1 to 5, it is characterised in that step 7) described in metal electrode be gold electrode, platinum electrode, tungsten electrode or nickel electrode；The thickness of metal electrode is 100nm.