An apparatus for nanofilm material electrode mask in diamond anvil cell and its using method

Abstract

The application relates to a device for electrode mask of nanometer thin film material in a diamond anvil cell and a use method thereof, and relates to the fields of mask plates and diamond anvil cell equipment, in particular to a device for electrode mask of nanometer thin film material in a diamond anvil cell and a use method thereof. The application aims to solve the technical problem that the preparation of nanometer thin film material electrodes in the existing diamond anvil cell is difficult. The device for electrode mask of nanometer thin film material in a diamond anvil cell is composed of a connecting plate, a diamond anvil cell, a metal frame, a positioning bolt, a vertical direction displacement table and a fixing bolt; the displacement of the diamond anvil cell in a horizontal plane and the up-down movement of the mask plate in the vertical direction are controlled, so that the mask plate and the thin-layer two-dimensional material can be precisely aligned in a three-dimensional space; in combination with the existing electron beam evaporation or thermal evaporation equipment, the nanometer thin film material can be conveniently electrode designed and prepared on the anvil surface of the diamond anvil cell.

Description

Technical Field

[0001] This invention relates to the field of mask plates and diamond anvil cell devices, and in particular to an apparatus for masking nanofilm materials in a diamond anvil cell and its method of use. Background Technology

[0002] Unlike traditional methods of applying uniaxial or biaxial pressure, diamond anvil cells can apply isotropic ultra-high hydrostatic pressure. During compression, the sample is placed in a pressure transmission medium within a gasket. The pressure applied to the gasket by the compressed diamond anvil cell is transmitted to the sample through the pressure transmission medium, resulting in uniform stress in all three-dimensional space. Understanding the properties of materials under high pressure is crucial, from condensed matter theory to novel chemical bonds and superconductivity. In isotropic ultra-high pressure environments, samples undergo structural transformations, affecting their physical and chemical properties.

[0003] With the continuous development of materials science, nanofilm materials, mainly two-dimensional materials, have shown broad application prospects in electronics, energy, optics and other fields due to their unique physical and chemical properties. Many two-dimensional materials and van der Waals heterostructures exhibit rich electronic properties under high pressure, such as pressure-induced superconductivity and topological phase transitions in van der Waals quantum spin Hall (QSH) insulators and twisted bilayer graphene (tBLG). By controlling high pressure, the performance of two-dimensional material devices can be optimized, such as improving key parameters like carrier mobility and fluorescence quantum yield, in order to obtain multifunctional materials with excellent superconducting properties and explore new physical phenomena and device applications. However, the study of the electrical properties of nanofilm materials, mainly two-dimensional materials, is limited by the difficulty in fabricating electrodes in diamond anvil cells. There is a lack of relevant technologies or equipment to achieve non-destructive metal electrode fabrication, making it impossible to achieve high-efficiency in-situ high-voltage electrical testing. Summary of the Invention

[0004] The present invention aims to solve the technical problem of the difficulty in preparing nanofilm material electrodes in existing diamond anvil cells, and provides a device and method for using a mask for nanofilm material electrodes in diamond anvil cells.

[0005] The device for electrode masking nanofilm materials in diamond anvil cells of the present invention consists of a connecting plate 4, a diamond anvil cell device 5, a metal frame 6, positioning bolts 7, a vertical displacement stage 8, and fixing bolts 9.

[0006] The connecting plate 4 is composed of two vertically connected flat plates, wherein the upper plate is placed vertically and the lower plate is placed horizontally.

[0007] The diamond anvil cell device 5 includes a diamond anvil cell 3;

[0008] The metal frame 6 is a hollow cylindrical structure with an open top and a bottom surface. The inner diameter of the metal frame 6 is larger than the outer diameter of the diamond anvil device 5. Four positioning bolts 7 of equal height are evenly arranged on the side wall of the metal frame 6 near the bottom. The positioning bolts 7 pass through the side wall of the metal frame 6 and are threadedly connected to the side wall of the metal frame 6.

[0009] The vertical displacement stage 8 is fixed above the metal frame 6; the vertical plate located above the connecting plate 4 is fixed to the moving part of the vertical displacement stage 8 by fixing bolts 9.

[0010] The vertical displacement stage 8 described in this invention is an existing device. As long as it can move up and down in a vertical direction, it is not the inventive point of this invention.

[0011] The method of using the device for electrode masking nanofilm materials in diamond anvil cells according to the present invention is as follows:

[0012] First, the bulk crystal of the two-dimensional material is peeled off by mechanical exfoliation to obtain a thin layer of two-dimensional material 1; then, the thin layer of two-dimensional material 1 is pasted and copied onto the surface of the PDMS film.

[0013] 2. Using a transfer table and a dry transfer method, the thin two-dimensional material 1 located on the surface of the PDMS film in step 1 is transferred to the anvil surface (i.e., the top plane of the diamond anvil 3) of the diamond anvil device 5. The thin two-dimensional material 1 is tightly attached to the anvil surface of the diamond anvil 3, and the PDMS film is on top. After standing and bonding for 3 to 5 minutes, the PDMS film is lifted to separate the PDMS film and the thin two-dimensional material 1. The thin two-dimensional material 1 and the anvil surface of the diamond anvil 3 are still tightly attached.

[0014] 3. Place the diamond anvil cell device 5 mentioned above in the inner cavity of the metal frame 6, and then attach the edge of the mask plate 2 to the lower surface of the horizontal lower plate of the connecting plate 4 through a new PDMS film.

[0015] Fourth, the vertical displacement stage 8 is controlled to move the connecting plate 4 vertically downwards. At the same time, the mask plate 2 and the thin two-dimensional material 1 are observed through the long working distance objective lens of the stereo microscope. When the mask plate 2 is close to the thin two-dimensional material 1, that is, when the mask plate 2 and the thin two-dimensional material 1 are about to be on the same focal plane, the vertical displacement of the connecting plate 4 is stopped. Then, the diamond anvil device 5 is adjusted in the horizontal plane within the metal frame 6 by rotating the four positioning bolts 7, so that the thin two-dimensional material 1 and the mask plate 2 are precisely aligned.

[0016] 5. Control the vertical displacement stage 8 to slowly lower the connecting plate 4 so that the thin two-dimensional material 1 and the mask plate 2 are attached. Use the cut high-temperature tape to stick and fix the mask plate 2 to the diamond anvil 3 so that the mask plate 2 and the thin two-dimensional material 1 are completely attached. Then, control the vertical displacement stage 8 to slowly raise the connecting plate 4 so that the connecting plate 4 and the mask plate 2 are separated, while the mask plate 2 and the thin two-dimensional material 1 remain on the diamond anvil 3.

[0017] 6. Place the diamond anvil cell device 5 mentioned above into a thermal evaporation or electron beam evaporation device to deposit metal electrodes.

[0018] This invention relates to the electrode preparation process for in-situ high-voltage electrical testing of nanofilm materials, and can be used to fabricate multi-electrode diamond anvil cell electrical devices. By controlling the displacement of the diamond anvil cell 3 in the horizontal plane and the vertical movement of the mask 2, this invention enables precise alignment of the mask 2 and the thin two-dimensional material 1 in three-dimensional space. Combined with existing electron beam evaporation or thermal evaporation equipment, electrodes for nanofilm materials can be conveniently designed and fabricated on the anvil surface of the diamond anvil cell 3. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the device used for the electrode mask of nanofilm material in a diamond anvil cell in Specific Implementation Method 7.

[0020] Figure 2 for Figure 1 First top view of the middle section of the structure;

[0021] Figure 3 for Figure 1 Second top view of the middle section structure;

[0022] Figure 4 This is a schematic diagram of the vertical displacement stage 8 in the first specific implementation method;

[0023] Figure 5 This is a top view of the diamond anvil cell 3 after vapor deposition in Experiment 1, at which point the mask 2 has been removed;

[0024] Figure 6 This is a three-dimensional schematic diagram of the diamond anvil cell 3 after vapor deposition in Experiment 1. At this point, the mask 2 has been removed. Detailed Implementation

[0025] Specific Implementation Method 1: This implementation method is a device for an electrode mask of nanofilm material in a diamond anvil cell, such as... Figures 1-6 As shown, it is specifically composed of a connecting plate 4, a diamond anvil device 5, a metal frame 6, positioning bolts 7, a vertical displacement stage 8, and fixing bolts 9;

[0026] The connecting plate 4 is composed of two vertically connected flat plates, wherein the upper plate is placed vertically and the lower plate is placed horizontally.

[0027] The diamond anvil cell device 5 includes a diamond anvil cell 3;

[0028] The metal frame 6 is a hollow cylindrical structure with an open top and a bottom surface. The inner diameter of the metal frame 6 is larger than the outer diameter of the diamond anvil device 5. Four positioning bolts 7 of equal height are evenly arranged on the side wall of the metal frame 6 near the bottom. The positioning bolts 7 pass through the side wall of the metal frame 6 and are threadedly connected to the side wall of the metal frame 6.

[0029] The vertical displacement stage 8 is fixed above the metal frame 6; the vertical plate located above the connecting plate 4 is fixed to the moving part of the vertical displacement stage 8 by fixing bolts 9.

[0030] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the metal frame 6 is made of stainless steel. Everything else is the same as in Specific Implementation Method One.

[0031] Specific Implementation Method Three: This implementation method differs from Specific Implementation Method One or Two in that the connecting plate 4 is composed of two vertically connected rectangular plates. Everything else is the same as in Specific Implementation Method One or Two.

[0032] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that the vertical displacement stage 8 is manually controlled. Everything else is the same as in Specific Implementation Methods One to Three.

[0033] Specific Implementation Method Five: This implementation method differs from Specific Implementation Method Four in that the vertical displacement stage 8 is electrically controlled. Everything else is the same as in Specific Implementation Method Four.

[0034] Specific Implementation Method Six: This implementation method differs from Specific Implementation Method Five in that the vertical displacement platform 8 and the metal frame 6 are an integral structure. Everything else is the same as in Specific Implementation Method Five.

[0035] Specific Implementation Method Seven: This implementation method is the method of using the device for the electrode mask of nanofilm material in diamond anvil cell as described in Specific Implementation Method One, as follows:

[0036] First, the bulk crystal of the two-dimensional material is peeled off by mechanical exfoliation to obtain a thin layer of two-dimensional material 1; then, the thin layer of two-dimensional material 1 is pasted and copied onto the surface of the PDMS film.

[0037] 2. Using a dry transfer method on a transfer table, the thin two-dimensional material 1 located on the surface of the PDMS film in step 1 is transferred to the anvil surface of the diamond anvil 3 in the diamond anvil device 5. The thin two-dimensional material 1 is in close contact with the anvil surface of the diamond anvil 3, and the PDMS film is on top. After standing and bonding for 3 to 5 minutes, the PDMS film is lifted to separate the PDMS film and the thin two-dimensional material 1. The thin two-dimensional material 1 and the anvil surface of the diamond anvil 3 are still in close contact.

[0038] 3. Place the diamond anvil cell device 5 mentioned above in the inner cavity of the metal frame 6, and then attach the edge of the mask plate 2 to the lower surface of the horizontal lower plate of the connecting plate 4 through a new PDMS film.

[0039] Fourth, the vertical displacement stage 8 is controlled to move the connecting plate 4 vertically downwards. At the same time, the mask plate 2 and the thin two-dimensional material 1 are observed through the long working distance objective lens of the stereo microscope. When the mask plate 2 is close to the thin two-dimensional material 1, that is, when the mask plate 2 and the thin two-dimensional material 1 are about to be on the same focal plane, the vertical displacement of the connecting plate 4 is stopped. Then, the diamond anvil device 5 is adjusted in the horizontal plane within the metal frame 6 by rotating the four positioning bolts 7, so that the thin two-dimensional material 1 and the mask plate 2 are precisely aligned.

[0040] 5. Control the vertical displacement stage 8 to slowly lower the connecting plate 4 so that the thin two-dimensional material 1 and the mask plate 2 are attached. Use the cut high-temperature tape to stick and fix the mask plate 2 to the diamond anvil 3 so that the mask plate 2 and the thin two-dimensional material 1 are completely attached. Then, control the vertical displacement stage 8 to slowly raise the connecting plate 4 so that the connecting plate 4 and the mask plate 2 are separated, while the mask plate 2 and the thin two-dimensional material 1 remain on the diamond anvil 3.

[0041] 6. Place the diamond anvil cell device 5 mentioned above into a thermal evaporation or electron beam evaporation device to deposit metal electrodes.

[0042] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Method Seven in that the mechanical exfoliation method described in step one involves using a special blue film for mechanical exfoliation to peel off the bulk crystal of the two-dimensional material to obtain a thin layer of two-dimensional material 1, the thickness of which is 1 nm to 10 nm. Everything else is the same as in Specific Implementation Method Seven.

[0043] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Method Eight in that the mask plate 2 mentioned in step three is a linear dual-electrode mask plate or a cross-shaped four-electrode mask plate. Everything else is the same as in Specific Implementation Method Eight.

[0044] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Method Nine in that the thickness of the mask plate 2 mentioned in step three is 30μm to 100μm. Everything else is the same as in Specific Implementation Method Nine.

[0045] The invention was verified using the following experiments:

[0046] Experiment 1: This experiment describes a device for masking nanofilm materials as electrodes in diamond anvil cells, such as... Figures 1-6 As shown, it is specifically composed of a connecting plate 4, a diamond anvil device 5, a metal frame 6, positioning bolts 7, a vertical displacement stage 8, and fixing bolts 9;

[0047] The connecting plate 4 is composed of two vertically connected rectangular plates, with the upper plate placed vertically and the lower plate placed horizontally.

[0048] The diamond anvil cell device 5 includes a diamond anvil cell 3;

[0049] The metal frame 6 is a hollow cylindrical structure with an open top and a bottom surface. The inner diameter of the metal frame 6 is larger than the outer diameter of the diamond anvil device 5. Four positioning bolts 7 of equal height are evenly arranged on the side wall of the metal frame 6 near the bottom. The positioning bolts 7 pass through the side wall of the metal frame 6 and are threadedly connected to the side wall of the metal frame 6. The metal frame 6 is made of stainless steel.

[0050] The vertical displacement stage 8 is fixed above the metal frame 6 and the two are an integral structure. The vertical displacement stage 8 is manually controlled. The vertical plate located above the connecting plate 4 is fixed to the moving part of the vertical displacement stage 8 by fixing bolts 9.

[0051] The method of using the above-mentioned device for electrode masking of nanofilm materials in diamond anvil cells is as follows:

[0052] First, the bulk crystal of two-dimensional material MoS2 is exfoliated using a special blue film for mechanical exfoliation to obtain a thin layer of two-dimensional material 1 with a thickness of 1nm to 10nm; then, the thin layer of two-dimensional material 1 on the blue film is copied onto the surface of the PDMS film.

[0053] 2. Using a dry transfer method on a transfer stage, the thin two-dimensional material 1 located on the surface of the PDMS film in step 1 is transferred to the anvil surface of the diamond anvil 3 in the diamond anvil cell device 5. The thin two-dimensional material 1 is in close contact with the anvil surface of the diamond anvil 3, and the PDMS film is on top. After standing and bonding for 3 minutes, the PDMS film is lifted to separate the PDMS film and the thin two-dimensional material 1. The thin two-dimensional material 1 and the anvil surface of the diamond anvil 3 are still in close contact. The process of lowering and lifting the PDMS film should be as slow as possible to avoid damage to the thin MoS2 layer, resulting in cracks or bubbles, so as to maintain the integrity and high quality of the sample.

[0054] 3. Place the diamond anvil cell device 5 inside the metal frame 6, and then attach the edge of the mask plate 2 to the lower surface of the horizontal lower plate of the connecting plate 4 using a new PDMS film (note that the PDMS film needs to be cut to a sufficiently small size, and only a small portion of the mask plate 2 should be attached to ensure that the connecting plate 4 and the mask plate 2 can be separated later); the mask plate 2 is a cross-shaped four-electrode mask (e.g., Figure 2 As shown), the thickness of mask 2 is 50 μm;

[0055] Fourth, the vertical displacement stage 8 is controlled to move the connecting plate 4 vertically downwards. At the same time, the mask plate 2 and the thin two-dimensional material 1 are observed through the long working distance objective lens of the stereo microscope. When the mask plate 2 is close to the thin two-dimensional material 1, that is, when the mask plate 2 and the thin two-dimensional material 1 are about to be on the same focal plane, the vertical displacement of the connecting plate 4 is stopped. Then, the diamond anvil device 5 is adjusted in the horizontal plane within the metal frame 6 by rotating the four positioning bolts 7, so that the thin two-dimensional material 1 and the mask plate 2 are precisely aligned.

[0056] 5. Control the vertical displacement stage 8 to slowly lower the connecting plate 4 so that the thin two-dimensional material 1 and the mask plate 2 are attached. Use the cut high-temperature tape to stick and fix the mask plate 2 to the diamond anvil 3 so that the mask plate 2 and the thin two-dimensional material 1 are completely attached. Then, control the vertical displacement stage 8 to slowly raise the connecting plate 4 so that the connecting plate 4 and the mask plate 2 are separated, while the mask plate 2 and the thin two-dimensional material 1 remain on the diamond anvil 3.

[0057] VI. The diamond anvil cell device 5 described above is placed in a thermal evaporation device to prepare the electrode by evaporation. Cr metal is selected as the binder layer and Au as the conductive layer to prepare an Au / Cr metal electrode. The Cr thickness is 5 nm and the Au thickness is 70 nm, resulting in the following... Figure 5 and 6 The diagram shows a MoS2 four-electrode device with a diamond anvil cell 3.

Claims

1. A device for masking nanofilm materials in diamond anvil cells, characterized in that... The device for the electrode mask of nano-thin film material in diamond anvil cell consists of a connecting plate (4), a diamond anvil cell device (5), a metal frame (6), positioning bolts (7), a vertical displacement stage (8), and fixing bolts (9). The connecting plate (4) is composed of two vertically connected flat plates, wherein the upper plate is placed vertically and the lower plate is placed horizontally. The diamond anvil cell device (5) includes a diamond anvil cell (3); The metal frame (6) is a hollow cylindrical structure with an open top and a bottom surface. The inner diameter of the metal frame (6) is larger than the outer diameter of the diamond anvil device (5). Four positioning bolts (7) of equal height are evenly arranged on the side wall of the metal frame (6) near the bottom. The positioning bolts (7) pass through the side wall of the metal frame (6) and are threadedly connected to the side wall of the metal frame (6). The vertical displacement stage (8) is fixed above the metal frame (6); the vertical plate located above the connecting plate (4) is fixed to the moving part of the vertical displacement stage (8) by fixing bolts (9); The method of using the above-mentioned device for electrode masks of nanofilm materials in diamond anvil cells is as follows: First, the bulk crystal of the two-dimensional material is peeled off by mechanical peeling to obtain a thin layer of two-dimensional material (1); then the thin layer of two-dimensional material (1) is pasted and copied onto the surface of the PDMS film; 2. Using a transfer table, the thin two-dimensional material (1) located on the surface of the PDMS film in step 1 is transferred to the anvil surface of the diamond anvil (3) in the diamond anvil device (5) by a dry transfer method. The thin two-dimensional material (1) is closely attached to the anvil surface of the diamond anvil (3), and the PDMS film is located on top. After standing and bonding for 3 to 5 minutes, the PDMS film is lifted to separate the PDMS film and the thin two-dimensional material (1). The thin two-dimensional material (1) and the anvil surface of the diamond anvil (3) are still closely attached.

3. Place the diamond anvil cell device (5) mentioned above in the inner cavity of the metal frame (6), and then attach the edge of the mask plate (2) to the lower surface of the horizontal lower plate of the connecting plate (4) through a new PDMS film. Fourth, control the vertical displacement stage (8) to move the connecting plate (4) vertically downward. At the same time, observe the mask plate (2) and the thin two-dimensional material (1) through the long working distance objective lens of the stereo microscope. Stop the vertical displacement of the connecting plate (4) when the mask plate (2) is close to the thin two-dimensional material (1), that is, when the mask plate (2) and the thin two-dimensional material (1) are about to be on the same focal plane. Then, adjust the horizontal displacement of the diamond anvil device (5) in the metal frame (6) by rotating the four positioning bolts (7) so that the thin two-dimensional material (1) and the mask plate (2) are precisely aligned.

5. Control the vertical displacement stage (8) to slowly lower the connecting plate (4) so ​​that the thin two-dimensional material (1) and the mask plate (2) are attached. Use the cut high-temperature tape to stick and fix the mask plate (2) to the diamond anvil (3) so that the mask plate (2) and the thin two-dimensional material (1) are completely attached. Then, control the vertical displacement stage (8) to slowly raise the connecting plate (4) so ​​that the connecting plate (4) and the mask plate (2) are separated, while the mask plate (2) and the thin two-dimensional material (1) remain on the diamond anvil (3).

6. Place the diamond anvil cell device (5) mentioned above into a thermal evaporation or electron beam evaporation device to deposit metal electrodes.

2. The device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The metal frame (6) is made of stainless steel.

3. The device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The connecting plate (4) is composed of two rectangular plates connected vertically.

4. The device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The vertical displacement stage (8) is manually controlled.

5. The apparatus for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The vertical displacement stage (8) is electrically controlled.

6. The apparatus for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The vertical displacement stage (8) and the metal frame (6) are an integral structure.

7. The method of using the device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The mechanical peeling method described in step one is to use a special blue film for mechanical peeling to peel off the bulk crystal of the two-dimensional material to obtain a thin layer of two-dimensional material (1), the thickness of which is 1nm~10nm.

8. The method of using the device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The mask (2) mentioned in step three is a linear dual-electrode mask or a cross-shaped four-electrode mask.

9. The method of using the device for an electrode mask of nanofilm material in a diamond anvil cell according to claim 1, characterized in that... The thickness of the mask plate (2) mentioned in step three is 30μm~100μm.

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