A six-sided anvil press cavity, its high-pressure solid-state gate control method and equipment

Abstract

This invention provides a six-sided anvil pressing cavity, the six-sided anvil pressing cavity comprising: a hollow cylindrical shell, a pair of symmetrical anvils having a 45° angle of inclination, and a 6-sided anvil pressing cavity. ° The invention comprises a guide block with an inclined plane, a primary anvil arranged in pairs along three coordinate axes, a cubic block placed within the primary anvil, and a solid electrolyte device. A high-voltage solid-state gate control method and apparatus are also provided. This invention enables in-situ gate voltage control of the device under hydrostatic pressure of 8 GPa. Due to the small volume of the high-voltage cavity, it is easily combined with low-temperature and strong magnetic field environments, enabling in-situ real-time control of multiple physical quantities under comprehensive extreme conditions. This is of great help in further exploring intrinsic exotic physical phenomena in condensed matter physics and potential device applications.

Description

Technical Field

[0001] This invention belongs to the field of condensed matter physics technology, specifically relating to a six-sided anvil chamber, its high-voltage solid-state gate control method and device. Background Technology

[0002] Real-time and continuous manipulation of the properties of condensed matter materials is a pursuit of every materials researcher. However, due to limitations in research methods, our current ability to manipulate material properties is very limited. For example, we can alter the band structure of a material by applying high voltage without introducing additional charge carriers. On the other hand, we can continuously and in real-time control the charge carrier concentration within the material through doping and electrostatic field manipulation, and this control is related to the material's band structure. If these two manipulation methods could be combined, allowing for in-situ modification of the band structure and further continuous and real-time control of the charge carrier concentration, it would open up a new world for the exploration and potential applications of new materials.

[0003] Compared to traditional field-effect transistors (FETs), which manipulate material properties and explore novel electronic states by altering the carrier concentration of a material through an electric field—static charge doping—the newly developed solid-state ion conductor-based FETs can not only achieve state control by injecting lithium ions to change the carrier concentration of the system, but also embed lithium ions into the crystal lattice to change its crystal structure and obtain new metastable phases. This unique feature makes solid-state ion conductor-based FETs potentially have a wide range of applications, as they overcome the drawbacks of sample surfaces being covered by electrolytes and electrolytes solidifying under low temperature or high pressure. Furthermore, the size of the device can be controlled, making them suitable for expanding various in-situ detection techniques while simultaneously controlling materials, thus greatly broadening the research in the field of state control. Because the piston cylinder pressure chamber has a large sample chamber volume (4 mm inner diameter and 10 mm length) and can achieve a hydrostatic pressure environment of 3 GPa, there are some reports on gate voltage regulation under high pressure. However, due to the limitation of pressure, the studied material system has not shown significant changes. In order to further study the continuous evolution of material states under extreme environments, a new high-pressure testing technology is urgently needed to break through the current pressure bottleneck and achieve a more systematic and comprehensive understanding of condensed matter physics materials. Summary of the Invention

[0004] Therefore, the purpose of this invention is to overcome the defects in the prior art and provide a six-sided anvil cavity, a high-voltage solid-state gate control method and device thereof.

[0005] To achieve the above objectives, a first aspect of the present invention provides a six-sided anvil pressing cavity, the six-sided anvil pressing cavity comprising: a hollow cylindrical shell, a pair of symmetrically arranged anvils having a 45° angle of curvature, and a 6-sided anvil pressing cavity. °The inclined guide block, the primary anvils that are opposite each other along the three coordinate axes, the cube block placed in the primary anvil, and the solid electrolyte device.

[0006] According to the six-sided anvil cavity of the first aspect of the present invention, the material of the hollow cylindrical outer shell is selected from one or more of the following: beryllium copper, stainless steel, tungsten carbide; preferably beryllium copper;

[0007] The guide block is made of one or more of the following materials: stainless steel, tungsten carbide, beryllium copper, nickel-chromium-aluminum; preferably nickel-chromium-aluminum.

[0008] The material of the primary anvil is selected from one or more of the following: tungsten carbide, stainless steel, nickel-chromium-aluminum, cubic boron nitride, polycrystalline diamond; preferably tungsten carbide;

[0009] The cubic block is made of magnesium oxide and / or yalasite; and / or

[0010] The material of the solid electrolyte device is selected from one or more of the following: magnesium oxide, strontium titanate, calcium fluoride, silicon wafer, and solid lithium-ion conductor; preferably, it is a solid lithium-ion conductor.

[0011] According to the first aspect of the present invention, the six-sided anvil cavity is wherein the cube is a cube divided in half, and each of the six faces of the cube has a pyramid-shaped pit of equal size, so that the cube has a winged sealing edge.

[0012] According to a first aspect of the present invention, the solid electrolyte device has a rectangular cross-section, with the sample located at its center, and four external electrodes are disposed at the four corners of the solid electrolyte surface, and a gate voltage adjustable back electrode is disposed on the back side of the solid electrolyte device.

[0013] A second aspect of the present invention provides a high-voltage solid-state gate modulation method, wherein the method uses the six-sided anvil cavity described in the first aspect for high-voltage solid-state gate modulation.

[0014] According to a second aspect of the present invention, a high-voltage solid-state gate modulation method comprises the following steps:

[0015] (1) The sample to be tested is cleaved into a thin layer and transferred to a solid electrolyte device, and electrodes are fabricated on the sample using micro-nano fabrication technology;

[0016] (2) Fix the external test electrode with silver paste at the electrode plated on the surface of the solid electrolyte. After the silver paste solidifies, turn the sample over and place it. Fix the gate voltage control back electrode with silver paste on its back. After the silver paste is completely dry, adjust and place the electrode inside the hollow cylindrical capsule fixed in the center of the half-divided cube. Fix the external test electrode. Then lead out the gate voltage control back electrode diagonally so that it is located in the gap between the two hammers. Fill the capsule with liquid pressure transmission medium and restore the half-divided cube into a complete cube block.

[0017] (3) Place the sealed edge of the cubic block from step (2) into the center of the first-level anvil embedded inside the upper and lower guide blocks, and fix the upper and lower guide blocks;

[0018] (4) Place the guide block inside the hollow cylindrical shell of the six-sided anvil pressure chamber, apply pressure and lock the pressure;

[0019] (5) After the pressure is locked, the six-sided anvil chamber is placed in a low-temperature thermostat. The carrier doping concentration is adjusted by locking different pressures and adjusting the voltage source at room temperature to complete the measurement.

[0020] According to the high voltage solid-state gate modulation method of the second aspect of the present invention, in step (1), the thickness of the thin layer is 10 ~ 50 nm, preferably 20 ~ 30 nm.

[0021] According to the high-voltage solid-state gate modulation method of the second aspect of the present invention, the material of the external test electrode and / or the gate voltage modulation back electrode is selected from one or more of the following: gold wire, platinum wire, enameled wire, preferably gold wire and / or platinum wire; and / or

[0022] The liquid pressure transmission medium is selected from one or more of the following: glycerol, Daphene 7373, Daphene 7474, silicone oil, and a mixture of methyl ethanol, preferably glycerol.

[0023] According to the high-voltage solid-state gate control method of the second aspect of the present invention, in step (4), the locking pressure is 0.7~8 GPa.

[0024] A third aspect of the present invention provides a state control device, the device comprising the six-sided anvil chamber described in the first aspect.

[0025] This invention is based on a six-sided anvil cavity to achieve 8GPa high-voltage solid-state gate modulation technology. This technology can be used to conduct systematic and in-depth in-situ high-voltage and carrier modulation research in the fields of condensed matter physics and materials science, accelerate the acquisition of more intrinsic material properties under comprehensive modulation conditions in materials science research, and provide important information for exploring new materials and designing new devices.

[0026] Solid-state electrolyte field-effect transistors (SFETs) not only allow for continuous manipulation of the material's state of matter by altering carrier concentration, but also enable lithium-ion intercalation, thereby changing the crystal structure to obtain new metastable phases that cannot be synthesized under conventional conditions. This unique characteristic significantly expands the scope of research in the field of state-of-the-art manipulation. Furthermore, SFETs overcome the drawback of liquid electrolytes covering the sample surface, making them suitable for in-situ measurements using various detection techniques to gain a deeper understanding of related physical processes. On the other hand, high pressure, as an independent thermodynamic parameter, can influence the crystal structure, interatomic interactions, and electron correlations of condensed matter, allowing for in-depth research into the material state, phase transition processes, phase transition mechanisms, and electronic dynamics of condensed matter under extreme conditions. Since electrons have multiple degrees of freedom, including spin, orbit, and charge, the balance between these interactions can be controlled by pressure. At the same time, with the addition of continuous charge carrier control, the comprehensive control of multiple physical quantities can be broadened, thereby realizing the distinctly different microscopic quantum ground states of the material itself. This will deepen our understanding of the mechanisms of different types of quantum phase transitions and provide a platform for further exploration of practical quantum phenomena, which will help open up a new world of materials applications.

[0027] The six-sided anvil pressing cavity of the present invention can have, but is not limited to, the following beneficial effects:

[0028] This invention enables in-situ gate voltage regulation of devices under hydrostatic pressure of 8 GPa. Due to the small volume of the high-voltage cavity, it is easy to combine with low temperature and strong magnetic field environments, and can realize in-situ real-time property regulation of multiple physical quantities under comprehensive extreme conditions. This is of great help for further exploration of intrinsic exotic physical phenomena in condensed matter physics and potential device applications. Attached Figure Description

[0029] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings, wherein:

[0030] Figure 1 The diagram shows a schematic of the various parts of a six-sided anvil cavity high-voltage solid-state gate control method and device, in which... Figure 1 (a) shows a schematic diagram of a solid-state ion conductor field-effect transistor device. Figure 1 (b) illustrates the standard four-electrode method for resistivity testing of FeSe thin-layer samples. Figure 1 (c) shows a test diagram of a solid-state ion-conducting field-effect transistor device with gold wires as electrodes fixed to them with silver paste. Figure 1 (d) shows a sample assembly diagram of a solid-state ion conductor field-effect transistor device. Figure 1 (e) shows a schematic diagram of the triaxial pressurization method of the cubic hexagonal anvil high-pressure chamber. Figure 1(f) shows an assembly diagram of the cubic hexagonal anvil high-pressure chamber sealing block, hammer head, and guide block. Figure 1 (g) shows the beryllium copper hollow cylindrical shell of a miniature six-sided anvil chamber. Figure 1 (h) shows a cross-sectional schematic diagram of the micro hexagonal anvil chamber after assembly.

[0031] Figure 2 The transport results of FeSe samples under in-situ multi-physical quantity modulation using the six-sided anvil cavity high-voltage solid-state gate modulation method in Experimental Example 1 are shown. Figure 2 a and Figure 2 b shows the control results at P=2 GPa and P=4 GPa, respectively.

[0032] Explanation of reference numerals in the attached figures:

[0033] 1. Support column; 2. Screw; 3. Support O-ring; 4. Support housing; 5. Hammer head fixed to the guide block; 6. Hammer head; 7. Beryllium copper hollow cylindrical shell of miniature six-sided anvil chamber; 8. Screw for fixing the guide block; 9. Spacer; 10. Guide block. Detailed Implementation

[0034] The present invention will be further illustrated below with specific embodiments. However, it should be understood that these embodiments are merely for more detailed and specific illustration and should not be construed as limiting the present invention in any way.

[0035] This section provides a general description of the materials and testing methods used in the experiments of this invention. While many of the materials and methods of operation used to achieve the objectives of this invention are well known in the art, the invention is still described in as much detail as possible herein. It will be apparent to those skilled in the art that, unless otherwise stated in the context, the materials and methods of operation used in this invention are well known in the art. Example 1

[0036] This embodiment is used to illustrate the structure of the six-sided anvil pressing cavity of the present invention.

[0037] The core module of the six-sided anvil chamber of the present invention includes the following parts: (1) a beryllium copper hollow cylindrical shell 7 of the micro six-sided anvil chamber; as shown in the attached figure. Figure 1 (g) shows the beryllium copper hollow cylindrical shell 7 of the micro hexagonal anvil chamber. In this embodiment, its overall height is 190mm and its diameter is 110mm. It is made of beryllium copper, material model: C1720BHT.

[0038] (2) A pair of symmetrical ones with 45 ° Guide block 10 of the inclined plane; as attached Figure 1(f) shows a pair of symmetrical guide blocks 10 with 45° inclined surfaces for a micro hexagonal anvil chamber. In this embodiment, the diameter is 80 mm and the height is 40 mm. The guide blocks are made of nickel-chromium-aluminum alloy or beryllium-copper alloy, preferably nickel-chromium-aluminum alloy.

[0039] (3) Six tungsten carbide primary anvils are arranged in pairs along the three coordinate axes; as shown in the attached figure. Figure 1 (e) shows the six tungsten carbide primary anvils of the micro hexagonal anvil chamber. In this embodiment, the upper and lower pairs of anvils have a cuboid base with a side length of 21 mm and a height of 20 mm; the front, back, left and right sides have four identical wedge-shaped anvils with a width of 25 mm and a length of 26.6 mm from the anvil surface to the tail of the anvil, and their backs are inclined surfaces with a 45° angle.

[0040] (4) A medium-density magnesium oxide cube or yerratum cube placed inside the primary anvil; the cube is a cube divided in half, and pyramid-shaped pits of equal size and appropriate depth are dug out on the six faces of the cube, so that the cube has a winged sealing edge.

[0041] (5) A specially designed solid electrolyte device, wherein the thin-layer sample is located at the center of the solid electrolyte. A designed mask allows for a large contact area between the four test electrodes and the solid electrolyte, resulting in high adhesion strength when the gold wire is fixed with silver paste as an external test electrode. The electrodes will not detach from the device during pressurization. The solid electrolyte can be made of a material with high lithium-ion mobility, preferably Li. 1+x+y Al x (Ti 2-y Ge y )P 3-z Si z O 12 .

[0042] The six-sided anvil cavity based on the present invention can realize high-voltage solid-state gate modulation technology of 8GPa.

[0043] Experimental Example 1

[0044] This embodiment is used to illustrate the high-voltage solid-state gate modulation method based on a six-sided anvil cavity of the present invention.

[0045] The high-voltage solid-state gate modulation technology based on a six-sided anvil cavity to achieve 8GPa is achieved by assembling the core module in the following manner:

[0046] 1. First, the sample to be tested is cleaved into thin layers of 10nm-30nm and transferred to a solid electrolyte substrate. Electrodes are then fabricated on the sample using micro / nano fabrication techniques such as electron beam lithography and photolithography. The test electrodes are fabricated into specially designed shapes, as shown in the attached figure. Figure 1As shown in (c), it is designed to facilitate in-situ testing by placing it into a six-sided anvil chamber.

[0047] 2. Gold wire leads are fixed to the electrode areas on the solid electrolyte surface using silver paste as the external electrodes for the standard four-electrode test. After the silver paste solidifies, the sample is flipped over, and another gold wire is fixed to its back using silver paste as the gate voltage control back electrode. In this solid electrolyte device, the four vapor-plated chromium-gold electrodes are located at the four corners of a wider rectangular cross-section, providing more electrode space. This ensures a more secure fixation of the gold wires and vapor-plated chromium-gold electrodes with silver paste, preventing the external electrodes from detaching from the solid electrolyte device during high-voltage application. During testing, five gold wires are used as electrodes. Four gold wires serve as the external electrodes for sample resistance testing on one side, while the gate voltage electrodes are located on the upper and lower surfaces of the solid electrolyte. One of the test electrodes on the upper surface serves as the gate voltage electrode test line. After the silver paste has completely dried, the five gold wire electrodes are positioned ideally and placed inside the hollow cylindrical Teflon capsule fixed in the center of the halved magnesium oxide cube. The Teflon capsule has an inner diameter of 2mm and a height of 3mm. The center of the halved cube has a cylindrical hole matching the size of the Teflon capsule, which can be glued into the hole. The external electrodes for testing the sample signal are then fixed in the following order: current negative electrode, voltage negative electrode, voltage positive electrode, current positive electrode, and gate voltage back electrode. The gate voltage control back electrode is then led out diagonally, located in the gap between the two hammers 6. Here, the five electrodes are identical except for their function and position. Finally, the Teflon capsule is filled with a liquid pressure-transmitting medium (a mixture of glycerol / Daphne 7373 / Daphne 7474 / silicone oil / methyl ethanol), and the halved cube is restored to a complete cube.

[0048] 3. Place the sealed edge of the cube block into the center of the 6 pressing anvils embedded inside the upper and lower guide blocks 10, and fix the upper and lower guide blocks 10 with two long screws 8.

[0049] 4. Place the guide block inside the beryllium copper hollow cylindrical shell of the miniature six-sided anvil pressure chamber. Place a pad 9 on the top of the guide block, tighten the top screw 2, and insert a cylindrical support column 1. Then, place the beryllium copper hollow cylindrical shell of the miniature six-sided anvil pressure chamber into the support O-ring 3, and place the support O-ring 3 on top of the support housing 4. Finally, place it in a press that can precisely control the oil pressure and slowly pressurize it. Finally, tighten the top screw 2 with a wrench to lock in a hydrostatic pressure of more than 8 GPa.

[0050] 5. After the pressure is locked, place it in a cryostat with a test temperature range of 1.5K-300K. At room temperature, the carrier doping concentration can be adjusted in real time using a voltage source. The material is then rapidly cooled to a low temperature while its resistance is measured simultaneously. By locking different pressures and adjusting the carrier concentration at room temperature, the performance of condensed matter physics materials can be continuously controlled in real time using multiple physical quantities.

[0051] The present invention was used to analyze the FeSe sample device under different pressures in Experiment Example 1, and the results are as follows: Figure 2 As shown. By Figure 2 a and Figure 2 As can be seen from b, without a gate voltage, the superconducting transition temperature of the FeSe sample device gradually increases with increasing pressure. It is approximately 8 K at ambient pressure, rising to 14 K at 2 GPa, and reaching 21 K at 4 GPa. When the gate voltage is adjusted between 2 GPa and 4 GPa, the superconducting transition temperature initially increases significantly with increasing gate voltage. When optimal superconductivity is achieved, the superconducting transition temperature decreases significantly with further increases in gate voltage. At a certain voltage value, its resistance exhibits semiconductor or insulator behavior. On one hand, applying high voltage can effectively change the lattice constant of the sample, thereby controlling the competitive interactions and Fermi surface electronic structure within the sample. On the other hand, applying an electric field to the solid lithium-ion conductor can effectively drive lithium ions in and out of the sample, thus achieving the control of the sample's physical properties. This invention enables systematic and in-depth in-situ high-pressure and carrier control studies of different material systems in the fields of condensed matter physics and materials science. This will accelerate the acquisition of more intrinsic material properties under comprehensive control conditions in materials science research, providing important information for exploring new materials and designing new devices.

[0052] Although the invention has been described to a certain extent, it is apparent that appropriate variations can be made to the various conditions without departing from the spirit and scope of the invention. It is understood that the invention is not limited to the described embodiments, but falls within the scope of the claims, which include equivalent substitutions for each of the elements.

Claims

1. A six-sided anvil pressing cavity, characterized in that, The six-sided anvil chamber includes: a hollow cylindrical shell, a pair of symmetrical anvils with 45° angles. ° The inclined guide block, the primary anvils that are opposite each other along the three coordinate axes, the cubic block placed in the primary anvil, and the solid electrolyte device; Wherein: the cube is a cube divided in half, and each of the six faces of the cube has a pyramid-shaped pit of equal size carved out, giving the cube a winged sealing edge; the solid electrolyte device has a rectangular cross-section, with the sample located at its center, and four external electrodes are set at the four corners of the solid electrolyte surface, and a gate voltage-controlled back electrode is set on the back of the solid electrolyte device; and the solid electrolyte is placed inside a hollow cylindrical capsule fixed in the center of the divided cube.

2. The six-sided anvil pressing cavity according to claim 1, characterized in that, The material of the hollow cylindrical shell is selected from one or more of the following: beryllium copper, stainless steel, and tungsten carbide.

3. The six-sided anvil pressing cavity according to claim 2, characterized in that, The hollow cylindrical shell is made of beryllium copper.

4. The six-sided anvil pressing cavity according to claim 1, characterized in that, The guide block is made of one or more of the following materials: stainless steel, tungsten carbide, beryllium copper, and nickel-chromium-aluminum.

5. The six-sided anvil pressing cavity according to claim 4, characterized in that, The guide block is made of nickel-chromium-aluminum.

6. The six-sided anvil pressing cavity according to claim 1, characterized in that, The material of the primary anvil is selected from one or more of the following: tungsten carbide, nickel-chromium-aluminum, stainless steel, cubic boron nitride, and polycrystalline diamond.

7. The six-sided anvil pressing cavity according to claim 6, characterized in that, The material of the primary anvil is tungsten carbide.

8. The six-sided anvil pressing cavity according to claim 1, characterized in that, The cubic block is made of magnesium oxide and / or yellow stone.

9. The six-sided anvil pressing cavity according to claim 1, characterized in that, The solid electrolyte device is made of one or more of the following materials: magnesium oxide, strontium titanate, calcium fluoride, silicon wafer, and solid lithium-ion conductor.

10. The six-sided anvil pressing cavity according to claim 9, characterized in that, The solid electrolyte device is made of solid lithium-ion conductor.

11. A high-voltage solid-state gate modulation method, characterized in that, The method employs a six-sided anvil cavity as described in any one of claims 1 to 10 for high-voltage solid-state gate modulation.

12. The high-voltage solid-state gate modulation method according to claim 11, characterized in that, The method includes the following steps: (1) The sample to be tested is cleaved into a thin layer and transferred to a solid electrolyte device, and electrodes are fabricated on the sample using micro-nano fabrication technology; (2) Fix the external test electrode with silver paste at the electrode plated on the surface of the solid electrolyte. After the silver paste solidifies, turn the sample over and place it. Fix the gate voltage control back electrode with silver paste on its back. After the silver paste is completely dry, adjust and place the electrode inside the hollow cylindrical capsule fixed in the center of the half-divided cube. Fix the external test electrode. Then lead out the gate voltage control back electrode diagonally so that it is located in the gap between the two hammers. Fill the capsule with liquid pressure transmission medium and restore the half-divided cube into a complete cube block. (3) Place the sealed edge of the cubic block from step (2) into the center of the first-level anvil embedded inside the upper and lower guide blocks, and fix the upper and lower guide blocks; (4) Place the guide block inside the hollow cylindrical shell of the six-sided anvil pressure chamber, apply pressure and lock the pressure; (5) After the pressure is locked, the six-sided anvil chamber is placed in a low-temperature thermostat. The carrier doping concentration is adjusted by locking different pressures and adjusting the voltage source at room temperature to complete the measurement.

13. The method according to claim 12, characterized in that, In step (1), the thickness of the thin layer is 10 ~ 50 nm.

14. The method according to claim 13, characterized in that, In step (1), the thickness of the thin layer is 20 ~ 30 nm.

15. The method according to claim 12, characterized in that, In step (2), the material of the external test electrode and / or the gate voltage regulating back electrode is selected from one or more of the following: gold wire, platinum wire, enameled wire; and / or The liquid pressure transmission medium is selected from one or more of the following: glycerol, Daphene 7373, Daphene 7474, silicone oil, and a mixture of methyl ethanol.

16. The method according to claim 15, characterized in that, In step (2), the material of the external test electrode and / or the gate voltage control back electrode is gold wire and / or platinum wire.

17. The method according to claim 15, characterized in that, In step (2), the liquid pressure transmission medium is glycerol.

18. The method according to any one of claims 12 to 17, characterized in that, In step (4), the locking pressure is 0.7 ~ 8 GPa.

19. A state control device, characterized in that, The device includes a six-sided anvil chamber as described in any one of claims 1 to 10.

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