Liquid shaping with charged particle beams

CN115411349BActive Publication Date: 2026-11-03FEI CO
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Patent Information

Application Number
CN202210585446.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Priority Date
2021-05-28
Filing Date
2022-05-27
Publication Date
2026-11-03
Estimated Expiration
2042-05-27

AI Technical Summary

Technical Problem

Existing technologies for preparing and observing micro-batteries, especially those using liquid electrolytes, result in high system complexity and low efficiency, making it difficult to effectively control liquid flow using charged particle beams.

Method used

By irradiating ionic liquids with a focused charged particle beam under low pressure, controlling their flow, and using electro-optic and electromagnetic lenses for focusing, combined with the adjustment of temperature and current density, precise flow and deposition of the liquid in microstructures can be achieved.

Benefits of technology

This simplifies the fabrication and observation process of microcells, improves efficiency, reduces system complexity, and enables precise control and flow of liquid electrolytes in microstructures.

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Abstract

The invention relates to a method for preparing and / or processing a sample. The sample comprises at least one fluid, and the method comprises directing a beam of charged particles onto the at least one fluid and causing the at least one fluid to flow in response to the beam of charged particles being directed onto the at least one fluid. The invention also relates to a system and a computer program product for performing the method.
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Description

Technical Field

[0001] This invention relates to the fields of nanotechnology and micromachining. The invention further relates to a method for preparing and / or processing samples by irradiating an ionic liquid with a beam of charged particles and causing it to flow. Background Technology

[0002] Charged particle beams, such as electron beams and ion beams, are widely used in microscopy, imaging, site-specific analysis, deposition, and materials ablation. Specifically, ion beams are widely used in the semiconductor and nanotechnology industries to fabricate and / or modify microstructures such as microprocessors and microcells. These utilize the ability of ions in the ion beam to interact with the atoms of the material they irradiate, thereby emitting any photon, electron, ion, neutral atom, or molecule. Due to their short wavelengths (due to the higher mass of the constituent particles) and their (electrostatic) focusing ability, ion beams can be used for site-specific sputtering or milling of microscopic (or nanoscale) structures. Examples include gallium (Ga)... + Focused ion beams can be used to mill features on the order of 10 nm. This could be particularly advantageous in the fabrication of microprocessors or microcells.

[0003] Specifically, focused ion beams are commonly used to fabricate and / or repair integrated circuits. The focused ion beam, often used in conjunction with a precursor gas, can be used to deposit microlayers, such as conductive metal layers, on a substrate. In the field of microcells, charged particle beams are used not only for in-situ observation of these microcells but also for their fabrication. However, their use in fabricating microcells is limited and primarily applied to solid-state batteries, where both the electrodes and electrolyte are solid. Solid-state batteries may require more complex fabrication systems and may be unstable within certain temperature ranges. Therefore, the use of liquid electrolytes in microcells is preferred. Liquid electrolytes that can be used for such microcells can include liquid metals or ionic liquids.

[0004] Ionic liquids are salts with low melting points (e.g., below 100°C) and typically low vapor pressures, making them particularly suitable as electrolytes in micro or nanocells. Due to their low vapor pressures, these salts remain liquid even at low pressures, allowing for in-situ observation of microcells using electron or ion beam microscopy, typically in the range of 10⁻⁶ Ω·cm. -5 Pa to 10 -2 Operates under pressure of Pa.

[0005] Typically, liquid electrolytes can be introduced into microcells using liquid injection systems that allow the electrolyte to be pumped between two microscopic (or nanoscale) electrodes. For example, Randolph et al., encapsulation-free fluid delivery and beam-induced electrodeposition in scanning electron microscopy (SEM) Capsule-free fluid delivery and beam- induced electrodeposition in a scanning electron microscope The paper "Progress in RSC (RSCAdv.)," 2013, 3, 20016, demonstrated the use of nanocapillaries to deliver an aqueous electrolytic copper sulfate (CuSO4) solution into the low-vacuum chamber of a scanning electron microscope. However, in addition to the microscope system used for observing the battery operation, a liquid injection system may also need to be installed. This can increase the complexity of the system and its failure rate. It may also reduce efficiency because different systems may need to be integrated and operated. Embodiments of the present invention aim to simplify and improve the efficiency of microbattery fabrication and observation.

[0006] Furthermore, embodiments of the present invention can also be used to prepare and / or process various samples, not limited to microcells. For example, it can be used to induce and / or control fluid flow, wherein the flow occurs on a substrate ranging in size from 1 µm to 1 cm. This may be relevant, for example, to any preparation, processing, and / or analysis of biological samples. Summary of the Invention

[0007] This invention relates to aspects that can be used to further improve the manufacture and / or analysis of microbatteries and their components, as well as corresponding methods. However, it should be understood that at least some of the embodiments described herein can also be used in fields different from battery systems.

[0008] This invention seeks to overcome or at least mitigate the shortcomings and deficiencies of the prior art. More specifically, the object of this invention is to provide an improved method, system, and computer program product for materials preparation and analysis.

[0009] An optional object of the present invention is to provide a system and method for preparing microscopic samples such as microbatteries. Specifically, an optional object of the present invention is to allow control of the flow of a liquid (such as an ionic liquid) by irradiating the liquid with a beam of charged particles.

[0010] In a first aspect, the present invention relates to a method for preparing and / or processing a sample, wherein the sample comprises at least one fluid, and wherein the method comprises directing a beam of charged particles onto the at least one fluid and causing the at least one fluid to flow in response to the directing of the charged particle beam onto the at least one fluid. The process may be carried out at, for example, a pressure range of 10... -5 Pa to 10 -2 The process is carried out in a low-pressure (high-vacuum) environment to minimize the interaction between charged particles in the charged particle beam and air molecules. This may help improve the efficiency of the process. In this case, the at least one fluid can be a liquid with a low vapor pressure.

[0011] The method may include guiding a beam of charged particles by focusing it. Focusing may be performed by a specialized assembly comprising electro-optical and / or electromagnetic lenses. For example, the focusing properties of the focusing assembly can be altered by changing the current in the electromagnetic lens, which changes the corresponding magnetic field.

[0012] The at least one fluid may include an electrical conductor.

[0013] The at least one fluid may include an ionic conductor.

[0014] The ionic conductor may include an ionic liquid.

[0015] The ionic liquid may include a low-temperature ionic liquid having a melting point equal to or below room temperature.

[0016] The ionic liquid may include organic cations such as 1-ethyl-3-methylimidazolium (EMIM), 1-butyl-3-methylimidazolium (BMIM), 1-octyl-3-methylimidazolium (OMIM), 1-decyl-3-methylimidazolium (DMIM), 1-butyl-2,3-dimethylimidazolium (DBMIM), 1-butyl-2,3-dimethylimidazolium (BMMIM), N-butyl-N-methylpyrrolidone (PYR14), N-methyl-N-propylpyrrolidone (PMPyr), N-methyl-N-propylpiperidinium (PP13), N-methyl-N-propylpyrrolidone (PYR13) or other organic cations.

[0017] At least one fluid as described above may include less than 10 -2 Pa, preferably less than 10 -5 Pa is the vapor pressure.

[0018] The viscosity of the at least one fluid can decrease as the temperature increases.

[0019] When the at least one fluid is heated from 25°C to 50°C, the viscosity of the at least one fluid decreases by at least 10% to at most 100% of its viscosity at 25°C. The viscosity dependence on temperature can be, for example, exponential, and its form is similar to the Arrhenius equation. The decrease in viscosity allows the at least one fluid to flow more easily, thereby enabling it to be positioned as needed.

[0020] The charged particle beam described above may include multiple charged particles.

[0021] The plurality of charged particles may include positively charged ions.

[0022] Alternatively, the plurality of charged particles may include electrons. Larger-mass ions can allow for better spatial resolution and greater momentum exchange with the constituent particles of at least one fluid. This, in turn, can contribute to improving the energy transfer efficiency from the charged particle beam to at least one fluid.

[0023] Positively charged ions can include any one of Ga, Xe, Ar, O, or N ions.

[0024] Multiple charged particles may comprise a beam, wherein the beam may be in the range of at least 1 pA to at most 100 µA, preferably in the range of at least 1 pA to at most 1 µA.

[0025] The method may further include focusing a charged particle beam onto at least one fluid and scanning throughout the fluid such that the charged particle beam current density is at least 5 fA / µm. 2 Up to 50 pA / µm 2 Within the range, preferably at least 0.05 pA / µm 2 Up to 5 pA / µm 2 Within a certain range. Lower current densities may be insufficient to induce fluid flow, while very high temperatures may damage the fluid, for example, through temperature-induced chemical changes. Therefore, the optimal current density can be selected / set based on the chemical composition of at least one fluid and the composition of the charged particle beam. The optimal current density can further depend on the energy of the charged particles in the charged particle beam. Furthermore, higher current densities can be used for lower energies of the charged particles.

[0026] The method may further include accelerating multiple charged particles within a beam of charged particles by applying a voltage.

[0027] The energies of the accelerated charged particles can range from at least 0.1 keV to at most 1 MeV. Higher energies may be particularly relevant when the method of the present invention is performed using a transmission electron microscope (TEM).

[0028] The method may further include transferring at least one fluid onto a substrate. The term "substrate" can be interpreted as any surface that can accommodate at least one fluid. For example, the substrate may correspond to the surface of a sample holder in a scanning electron microscope (SEM) system, in case the method is performed using an SEM. Alternatively, the substrate may be a specially designed holder for the purpose of performing the method.

[0029] The method may include transferring at least one fluid onto a substrate.

[0030] At least one fluid can be transferred onto a substrate using a pipette. For example, a pipette can deliver volumes ranging from at least 1 nL to 1 µL, or droplet sizes from 0.1 mm to 1 mm, and can itself have microscale dimensions.

[0031] The method may further include guiding a beam of charged particles to a scanning point on at least one fluid. For example, the scanning point may include a point where the charged particle beam can be focused. The scanning point may further correspond to an electron or ion point on the sample.

[0032] The method may further include scanning a charged particle beam across at least one fluid at multiple scanning locations in one, two, or three dimensions. For example, for the purpose of scanning in three dimensions, multiple charged particle beams may be used, such as each of the multiple charged particle beams scanning in two vertical planes. Alternatively, by controlling the energy of the charged particles in the charged particle beams, the effective depth of interaction can also be varied, thereby allowing for three-dimensional scanning of at least one fluid.

[0033] The method may include a charged particle beam at a concentration between 10... -10 meters per second and 10 7 Between meters per second, preferably between 10 -4 The surface of at least one fluid is scanned at a rate between m / s and 100 m / s. It should be understood that these rates may represent average and / or instantaneous rates at which a given surface area of ​​at least one fluid can be scanned. In other words, the scope of the invention can also be understood to correspond to the total time required to scan a specific surface region of at least one fluid.

[0034] The substrate described above can include any of silicon nitride (SiN), aluminum (Al), or any other material. For example, if at least one fluid corresponds to an electrolyte, this can allow, for example, a non-conductive substrate to be used to fabricate a microcell. For example, the current can then be measured by placing a pair of electrodes in contact with the electrolyte and establishing a voltage difference between the electrodes.

[0035] The sample may further include multiple conductive elements, such as two conductive elements.

[0036] The two conductive elements may include electrodes, such that one conductive element includes an anode and the other conductive element includes a cathode. Therefore, the two conductive elements may include the electrodes of a battery.

[0037] The size of the multiple conductive elements can range from at least 1 nm to at most 50 cm. Conductive elements at the smaller end of this range can enable the fabrication of nanocells using the method proposed in this invention, while larger cells can be achieved by using conductive elements at the other end of the range.

[0038] The two conductive elements described above can be positioned such that they are more than 1 nm apart.

[0039] The cathode may include any of the following: lithium titanate oxide (LTO), lithium nickel manganese cobalt oxide (NMC), lithium iron phosphate (LFP), lithium iron manganese phosphate (LFMP), lithium manganese oxide (LMO), lithium nickel manganese oxide (LNMO), lithium nickel cobalt aluminum oxide (NCA), lithium cobalt oxide (LCO), sulfur (S), or any other material used for cathodes in batteries. Specifically, the cathode may include any material used for cathodes in batteries having a liquid electrolyte.

[0040] The anode may include any of the following: lithium (Li), graphite, silicon, lithium titanate oxide (LTO), tin (Sn), or any other material used for anodes in batteries. Specifically, the anode may include any material used for anodes in batteries having a liquid electrolyte.

[0041] The result of scanning the charged particle beam across the at least one fluid at the scanning location may include the interaction between the charged particle beam and the at least one fluid. This interaction may be mechanical, resulting in the transfer of energy from the charged particle beam to the component particles (e.g., ions, atoms, or molecules) of the at least one fluid. This energy transfer may reduce the viscosity of the at least one fluid.

[0042] The result of the interaction between a charged particle beam and at least one fluid may include the flow of the at least one fluid through the substrate.

[0043] At least one fluid as described above may further include an electrolyte. As described above, if a potential difference is established between the multiple conductive elements, this can allow current to flow between the multiple conductive elements.

[0044] The method described above can further include lift-out and transfer steps. These steps can be performed to manufacture the multiple conductive elements described above.

[0045] The removal step may include milling and removing multiple conductive elements from multiple block samples. Typically, block samples of any material including conductive elements as described above can be used to manufacture the conductive elements.

[0046] The extraction step may include extracting the Li conductive element from the lithium bulk sample. It will be understood that bulk samples of any of the other materials described above may be used to extract the anode conductive element.

[0047] The extraction step may include extracting the LTO conductive element from the lithium titanate bulk sample. It is understood that bulk samples of any of the other materials described above can be used to extract the cathode conductive element.

[0048] The transfer steps described above may include transferring any conductivity from a plurality of conductive elements onto a substrate.

[0049] The step of transferring at least one fluid onto the substrate may precede the step of transferring any of the plurality of conductive elements onto the substrate. Alternatively, at least one of the conductive elements may be transferred onto the substrate, followed by the transfer of at least one fluid onto the substrate, and then the remaining conductive elements of the plurality of conductive elements may be further transferred onto the substrate.

[0050] The interaction between a charged particle beam and at least one fluid can result in the transfer of at least a portion of the fluid to a region on a substrate, wherein the region corresponds to a gap between two conductive elements. This can be advantageous in cases where the methods described herein are used to fabricate batteries, for example, where the at least one fluid can be used to provide a conductive path between multiple conductive elements. Controlling the flow of at least one fluid using a charged particle beam, as described above, allows even very small volumes of fluid (approximately 1 pL) to be accurately propelled into, for example, a space of approximately 10 µm between two conductive elements without requiring a separate liquid injection system in addition to the fabrication / imaging system.

[0051] Any of the multiple conductive elements described above can be transferred onto the substrate described above using a needle.

[0052] The needle may include a microneedle. When the conductive element has a nanoscale size, the needle may also include a nanoscale needle.

[0053] The substrate may include a sample holder. As described above, at least a portion of the sample holder may itself include the substrate, making it possible to eliminate the need for a separate substrate.

[0054] Sample holders may include SEM sample holders.

[0055] The sample holder may include multiple arms, such as two arms, each configured to provide conductive contact to at least one of the multiple conductive elements. For example, multiple arms can thus allow a voltage difference to be established between any of the multiple conductive elements with the aid of an external voltage source. This can be particularly advantageous when the conductive elements have nanoscale or microscale dimensions and connecting them to an external voltage source may require complex processes.

[0056] Each of the plurality of arms can be connected to a voltage source, such that a non-zero potential difference can be generated between any two of the plurality of arms.

[0057] The methods described above may include transferring any conduction from a plurality of conductive elements to any of the plurality of arms of a sample holder.

[0058] The method may further include monitoring the flow of the at least one fluid in response to a charged particle beam being directed onto the at least one fluid.

[0059] The method may further include applying a non-zero potential difference between the anode and the cathode and measuring the current between the anode and the cathode.

[0060] The method may further include stopping the flow of at least one fluid between the two conductive elements once a non-zero current is measured between the anode and the cathode.

[0061] Monitoring the flow of the at least one fluid may further include imaging the sample. Specifically, imaging the sample may be performed in parallel with any of the steps described above, including irradiating the at least one fluid with charged particles and / or lift-off and transfer steps. This can be particularly advantageous in terms of controlling each process (e.g., stop time) and can contribute to improving the efficiency of sample preparation and / or processing methods. Images may also be recorded by, for example, a data processing system, which may be used in conjunction with a system for performing the methods described herein.

[0062] Imaging a sample can include detecting emission caused by the interaction of a beam of charged particles with at least one fluid.

[0063] The emission can include photons, electrons, or ions. Electrons can include any of backscattered electrons, transmitted electrons, secondary electrons, or Auger electrons. Ions can include secondary ions. For example, photons can include a spectrum ranging from IR to X-rays.

[0064] Images may include SEM images, TEM images, and / or FIB images.

[0065] In a second aspect, the present invention relates to a system comprising a scanning microscope system and a data processing system, wherein the system is configured to process a sample, wherein the sample comprises at least one fluid, and wherein the system is configured to direct a beam of charged particles onto the at least one fluid and to cause the at least one fluid to flow in response to the beam of charged particles being directed onto the at least one fluid.

[0066] Guiding the charged particle beam may include focusing the charged particle beam.

[0067] Scanning microscope systems may include focused ion beam (FIB) microscopes.

[0068] The system, specifically the scanning microscope system, can be configured to scan the charged particle beam across the at least one fluid at multiple scanning points in one, two, or three dimensions.

[0069] The system, specifically the data processing system, can be further configured to assign a two-dimensional coordinate system to the sample.

[0070] The system described above can be configured to monitor the flow of the at least one fluid, wherein monitoring the flow of the at least one fluid may further include imaging the sample.

[0071] The system, specifically the scanning microscope system, can be further configured to image the sample by detecting emission generated by the interaction of the charged particle beam with the at least one fluid.

[0072] The system, specifically the data processing system, may include a data storage element, wherein the system may be configured to store an image of the sample in the data storage element.

[0073] The system may further include a display, and the system may be configured to display a sample image on the display.

[0074] The system, specifically the data processing system as described above, can be configured to allow an operator to monitor the flow of the at least one fluid based on the displayed images.

[0075] The system, specifically the data processing system described above, can be configured to control the scanning position of the charged particle beam in a coordinate system associated with the sample by controlling the direction of the charged particle beam.

[0076] The system, specifically the scanning microscope system described above, may include an electro-optic system configured to guide and / or focus the charged particle beam.

[0077] The system, specifically the data processing system as described above, can be further configured to control the electro-optic system, wherein the data processing system is configured to control the direction of the charged particle beam by controlling the electro-optic system.

[0078] The following will discuss embodiments of the method. Embodiments of the method are abbreviated as the letter "M" followed by a number. Whenever "method embodiment" is mentioned herein, it refers to these embodiments.

[0079] M1. A method for preparing and / or processing a sample, wherein the sample comprises at least one fluid; and wherein the method includes A charged particle beam is directed onto the at least one fluid and the at least one fluid is made to flow in response to the charged particle beam being directed onto the at least one fluid.

[0080] M2. The method according to the previous embodiment, wherein guiding the charged particle beam includes focusing the charged particle beam.

[0081] M3. The method according to any one of the foregoing embodiments, wherein the at least one fluid comprises an electrical conductor.

[0082] M4. The method according to any one of the foregoing embodiments, wherein the at least one fluid comprises an ion conductor.

[0083] M5. The method according to the previous embodiment, wherein the ionic conductor comprises an ionic liquid.

[0084] M6. The method according to the previous embodiment, wherein the ionic liquid includes a low-temperature ionic liquid having a melting point equal to or below room temperature.

[0085] M7. The method according to the preceding embodiment, wherein the ionic liquid comprises an organic cation, such as 1-ethyl-3-methylimidazolium (EMIM), 1-butyl-3-methylimidazolium (BMIM), 1-octyl-3-methylimidazolium (OMIM), 1-decyl-3-methylimidazolium (DMIM), 1-butyl-2,3-dimethylimidazolium (DBMIM), 1-butyl-2,3-dimethylimidazolium (BMMIM), N-butyl-N-methylpyrrolidone (PYR14), N-methyl-N-propylpyrrolidone (PMPyr), N-methyl-N-propylpiperidinium (PP13), N-methyl-N-propylpyrrolidone (PYR13) or other organic cations.

[0086] M8. The method according to any one of the foregoing embodiments, wherein the at least one fluid comprises less than 10 -2 Pa, preferably less than 10 -5 Pa is the vapor pressure.

[0087] M9. The method according to any one of the foregoing embodiments, wherein the viscosity of the at least one fluid decreases with increasing temperature.

[0088] M10. The method according to the previous embodiment, wherein when the at least one fluid is heated from 25°C to 50°C, the viscosity of the at least one fluid decreases by a range of at least 10% to at most 100% of the viscosity at 25°C.

[0089] M11. The method according to any one of the foregoing embodiments, wherein the charged particle beam comprises a plurality of charged particles.

[0090] M12. The method according to the previous embodiment, wherein guiding the plurality of charged particles includes positively charged ions.

[0091] M13. The method according to the penultimate embodiment, wherein the plurality of charged particles include electrons.

[0092] M14. The method according to the penultimate embodiment, wherein the positively charged ion includes any one of Ga, Xe, Ar, O, or N ions.

[0093] M15. A method according to any one of the foregoing embodiments and having the features of embodiment M11, wherein the plurality of charged particles comprise a beam, and wherein the beam is in the range of at least 1 pA to at most 100 µA, preferably in the range of at least 1 pA to at most 1 µA.

[0094] M16. The method according to the preceding embodiment, wherein the method further comprises focusing a charged particle beam onto at least one fluid and scanning throughout the fluid such that the charged particle beam current density is at least 5 fA / µm. 2 Up to 50 pA / µm 2 Within the range, preferably at least 0.05 pA / µm 2 Up to 5 pA / µm 2 Within the range.

[0095] M17. A method according to any one of the foregoing embodiments and having the features of embodiment M11, wherein the method includes accelerating the plurality of charged particles within the charged particle beam by applying a voltage.

[0096] M18. The method according to the previous embodiment, wherein the energy of the accelerated charged particles is in the range of at least 0.1 keV to at most 1 MeV.

[0097] M19. The method according to any one of the foregoing embodiments, wherein the method further comprises transferring the at least one fluid onto a substrate.

[0098] M20. The method according to the previous embodiment, wherein the method includes transferring the at least one fluid onto the substrate.

[0099] M21. The method according to the previous embodiment, wherein the at least one fluid is transferred onto the substrate via a pipette.

[0100] M22. The method according to any one of the foregoing embodiments, wherein the method further comprises guiding the charged particle beam to a scanning point on the at least one fluid.

[0101] M23. The method according to any one of the preceding embodiments, wherein the method further comprises scanning the charged particle beam across the at least one fluid at multiple scanning positions in one, two, or three dimensions.

[0102] M24. The method according to any one of the foregoing two embodiments, wherein the method comprises a charged particle beam at a concentration between 10... -10 meters per second and 10 7 Between meters per second, preferably between 10 -4 The surface of the at least one fluid is scanned at a rate between m / s and 100 m / s.

[0103] M25. A method according to any one of the foregoing embodiments and having the features of embodiment M19, wherein the substrate comprises any one of SiN, Al or any other material.

[0104] M26. The method according to any of the foregoing embodiments, wherein the sample further comprises a plurality of conductive elements, such as two conductive elements.

[0105] M27. The method according to the previous embodiment, wherein the two conductive elements include electrodes, such that one conductive element includes an anode and the other conductive element includes a cathode.

[0106] M28. The method according to any one of the preceding two embodiments, wherein the size of each of the plurality of conductive elements is in the range of at least 1 nm to at most 50 cm.

[0107] M29. The method according to any one of the preceding three embodiments, wherein the two conductive elements are positioned at a distance greater than 1 nm from each other.

[0108] M30. A method according to any of the foregoing embodiments and having the characteristics of embodiment M27, wherein the cathode comprises any lithium titanate (LTO).

[0109] M31. A method according to any one of the foregoing embodiments and having the features of embodiment M27, wherein the anode comprises lithium (Li).

[0110] M32. A method according to the preceding embodiment and having the features of embodiment M23, wherein the result of scanning the charged particle beam across the at least one fluid throughout the scanning position may include the interaction between the charged particle beam and the at least one fluid.

[0111] M33. A method according to the preceding embodiment and having the features of embodiment M19, wherein the result of the interaction between the charged particle beam and the at least one fluid includes the flow of the at least one fluid through the substrate.

[0112] M34. A method according to the previous embodiment and having the characteristics of embodiment M3, wherein the at least one fluid comprises an electrolyte.

[0113] M35. The method according to any one of the preceding claims, wherein the method further comprises a lift-off step and a transfer step.

[0114] M36. A method according to the previous embodiment and having the features of embodiment M26, wherein the lifting step includes milling and removing the plurality of conductive elements from a plurality of block samples.

[0115] M37. A method according to the preceding embodiment and having the features of embodiment M31, wherein the extraction step includes extracting Li conductive elements from a lithium bulk sample.

[0116] M38. A method according to any one of the foregoing two embodiments and having the characteristics of embodiment M30, wherein the extraction step comprises extracting the LTO conductive element from a lithium titanate bulk sample.

[0117] M39. A method according to any one of the foregoing embodiments and having the features of embodiments M19, M26 and M35, wherein the transfer step includes transferring any of the plurality of conductive elements onto the substrate.

[0118] M40. A method according to the preceding embodiment and having the features of embodiment M11, wherein the step of transferring the at least one fluid onto the substrate precedes the step of transferring any of the plurality of conductive elements onto the substrate.

[0119] M41. A method according to any one of the foregoing embodiments and having the features of embodiments M29, M23 and M39, wherein the result of the interaction between the charged particle beam and the at least one fluid includes transferring at least a portion of the fluid to a region on the substrate, wherein the region corresponds to the gap between the two conductive elements.

[0120] M42. A method according to any one of the foregoing embodiments and having the features of embodiment M39, wherein any of the plurality of conductive elements is transferred onto the substrate by means of a needle.

[0121] M43. The method according to the previous embodiment, wherein the needle includes a microneedle.

[0122] M44. A method according to any one of the foregoing embodiments and having the features of embodiment M19, wherein the substrate includes a sample holder.

[0123] M45. The method according to the previous embodiment, wherein the sample holder includes a SEM sample holder.

[0124] M46. A method according to any one of the foregoing two embodiments and having the features of embodiment M26, wherein the sample holder comprises a plurality of arms, such as two arms, each of the plurality of arms being configured to provide conductive contact to at least one of the plurality of conductive elements.

[0125] M47. The method according to the previous embodiment, wherein each of the plurality of arms is connected to a voltage source such that a non-zero potential difference can be generated between any two of the plurality of arms.

[0126] M48. A method according to any one of the foregoing three embodiments and having the features of embodiment M39, wherein transferring any of the plurality of conductive elements onto the substrate comprises transferring any conductive element onto any of the plurality of arms of the sample holder.

[0127] M49. The method according to any one of the foregoing embodiments, wherein the method further includes monitoring the flow of the at least one fluid in response to the charged particle beam being directed onto the at least one fluid.

[0128] M50. A method according to the preceding embodiment and having the features of embodiments M27 and M47, wherein the method further comprises applying a non-zero potential difference between the anode and the cathode and measuring the current between the anode and the cathode.

[0129] M51. The method according to the previous embodiment, wherein the method further includes stopping the flow of the at least one fluid between the two conductive elements once a non-zero current is measured between the anode and the cathode.

[0130] M52. A method according to any one of the foregoing embodiments and having the features of embodiment M49, wherein monitoring the flow of the at least one fluid further comprises imaging the sample.

[0131] M53. A method according to the previous embodiment and having the features of embodiment M33, wherein imaging the sample includes detecting emission caused by the interaction of the charged particle beam with the at least one fluid.

[0132] M54. The method according to the previous embodiment, wherein the emission comprises photons.

[0133] M55. The method according to any one of the foregoing two embodiments, wherein the emission comprises electrons.

[0134] M56. The method according to the previous embodiment, wherein the electron includes any one of backscattered electrons, transmitted electrons, secondary electrons, or Auger electrons.

[0135] M57. The method according to any one of the foregoing four embodiments, wherein the emission comprises ions.

[0136] M58. The method according to the previous embodiment, wherein the ion includes a secondary ion.

[0137] M59. A method according to any one of the foregoing embodiments and having the features of embodiment M55, wherein the image includes a SEM image.

[0138] M60. A method according to any one of the foregoing embodiments and having the features of embodiment M55, wherein the image includes a TEM image.

[0139] M61. A method according to any one of the foregoing embodiments and having the features of any one of embodiments M55 and M57, wherein the image includes a FIB image.

[0140] The following will discuss embodiments of the system. System embodiments are abbreviated as the letter "S" followed by a number. Whenever "system embodiment" is mentioned herein, it refers to these embodiments.

[0141] S1. A system comprising a scanning microscope system and a data processing system, wherein the system is configured to process a sample, wherein the sample comprises at least one fluid, and wherein the system is configured to • Directing a beam of charged particles onto the at least one fluid and causing the at least one fluid to flow in response to the beam of charged particles being directed onto the at least one fluid.

[0142] S2. The system according to the previous embodiment, wherein guiding the charged particle beam includes focusing the charged particle beam.

[0143] S3. The system according to any one of the foregoing system embodiments, wherein the at least one fluid comprises an electrical conductor.

[0144] S4. The system according to any one of the foregoing system embodiments, wherein the at least one fluid comprises an ion conductor.

[0145] S5. The system according to any one of the foregoing system embodiments, wherein the at least one fluid comprises an ionic liquid.

[0146] S6. The system according to the previous embodiment, wherein the ionic liquid includes a low-temperature ionic liquid having a melting point equal to or below room temperature.

[0147] S7. The system according to the previous embodiment, wherein the ionic liquid comprises 1-ethyl-3-methylimidazolium (EMIM), 1-butyl-3-methylimidazolium (BMIM), 1-octyl-3-methylimidazolium (OMIM), 1-decyl-3-methylimidazolium (DMIM), 1-butyl-2,3-dimethylimidazolium (DBMIM), 1-butyl-2,3-dimethylimidazolium (BMMIM), N-butyl-N-methylpyrrolidone (PYR14), N-methyl-N-propylpyrrolidone (PMPyr), N-methyl-N-propylpiperidinium (PP13), N-methyl-N-propylpyrrolidone (PYR13) or other organic cations.

[0148] S8. The system according to any one of the foregoing system embodiments, wherein the at least one fluid comprises less than 10 -2 Pa, preferably less than 10 -5 Pa is the vapor pressure.

[0149] S9. The system according to any one of the foregoing system embodiments, wherein the viscosity of the at least one fluid decreases as the temperature increases.

[0150] S10. The system according to the previous embodiment, wherein when the fluid is heated from 25°C to 50°C, the viscosity of the at least one fluid decreases by a range of at least 10% to at most 100% of the viscosity at 25°C.

[0151] S11. The system according to any one of the foregoing system embodiments, wherein the charged particle beam comprises a plurality of charged particles.

[0152] S12. The system according to the previous embodiment, wherein guiding the plurality of charged particles includes positively charged ions.

[0153] S13. The system according to the penultimate embodiment, wherein the plurality of charged particles include electrons.

[0154] S14. The system according to the penultimate embodiment, wherein the positively charged ion includes any one of Ga, Xe, Ar, O, or N ions.

[0155] S15. The system according to any one of the foregoing system embodiments, wherein the scanning microscope system includes a focused ion beam (FIB) microscope.

[0156] S16. A system according to any one of the foregoing system embodiments and having the features of embodiment S11, wherein the plurality of charged particles comprise a beam, and wherein the beam is in the range of at least 1 pA to at most 100 µA, preferably in the range of at least 1 pA to at most 1 µA.

[0157] S17. The system according to the preceding embodiment, wherein the system, specifically the scanning microscope system, is configured to focus a charged particle beam onto at least one fluid and scan throughout the fluid such that the charged particle beam current density is at least 5 fA / µm. 2 Up to 5 pA / µm 2 Within the range, preferably at least 0.05 pA / µm 2 Up to 5 pA / µm 2 Within the range.

[0158] S18. A system according to any one of the foregoing system embodiments and having the features of embodiment S11, wherein the system, specifically the scanning microscope system, is configured to accelerate the plurality of charged particles within the charged particle beam by applying a voltage.

[0159] S19. The system according to the previous embodiment, wherein the energy of the accelerated charged particles is in the range of at least 0.1 keV to at most 1 MeV.

[0160] S20. The system according to any one of the foregoing system embodiments, wherein the system, specifically the scanning microscope system, further includes a substrate.

[0161] S21. The system according to the previous embodiment, wherein the system, specifically the scanning microscope system, is configured to transfer the at least one fluid onto the substrate via a pipette.

[0162] S22. The system according to any one of the foregoing system embodiments, wherein the system, specifically the scanning microscope system, is further configured to guide the charged particle beam to a scanning point on the at least one fluid.

[0163] S23. The system according to any one of the preceding embodiments, wherein the system, specifically the scanning microscope system, is configured to scan a charged particle beam across at least one fluid at multiple scanning positions in one, two, or three dimensions.

[0164] S24. The system according to any one of the foregoing system embodiments, wherein the system, specifically the data processing system, is further configured to assign a two-dimensional coordinate system to the sample.

[0165] S25. The system according to any one of the foregoing two embodiments, wherein the system, specifically the scanning microscope system, is configured to cause the charged particle beam to be at a frequency between 10... -10 meters per second and 10 7 Between meters per second, preferably between 10 -4 A rate between 100 m / s and 100 m / s is used to scan the surface of the at least one fluid.

[0166] S26. A system according to any one of the foregoing system embodiments and having the features of embodiment S20, wherein the substrate comprises any one of SiN, Al or any other material.

[0167] S27. The system according to any one of the foregoing system embodiments, wherein the sample further comprises at least two or more conductive elements.

[0168] S28. The system according to the previous embodiment, wherein the two conductive elements include electrodes, such that one conductive element includes an anode and the other conductive element includes a cathode.

[0169] S29. The system according to any one of the foregoing two embodiments, wherein the size of each of the at least two conductive elements is in the range of at least 1 nm to at most 50 cm.

[0170] S30. The system according to any one of the three system embodiments described above, wherein the two conductive elements are positioned at a distance greater than 1 nm from each other.

[0171] S31. A system according to any one of the foregoing system embodiments and having the features of embodiment S28, wherein the cathode comprises lithium titanate (LTO).

[0172] S32. A system according to any of the foregoing system embodiments and having the features of embodiment S28, wherein the anode comprises lithium (Li).

[0173] S33. A system according to any of the foregoing system embodiments and having the features of embodiment S23, wherein the result of scanning the charged particle beam across the at least one fluid throughout the scanning position may include the interaction between the charged particle beam and the at least one fluid.

[0174] S34. A system according to the preceding embodiment and having the features of embodiment S20, wherein the result of the interaction between the charged particle beam and the at least one fluid includes the flow of the at least one fluid through the substrate.

[0175] S36. A system according to any one of the foregoing system embodiments and having the features of embodiment S27, wherein the system, specifically the scanning microscope system, is configured to mill and remove the at least two conductive elements from at least two corresponding bulk samples by means of the charged particle beam.

[0176] S37. The system according to any one of the foregoing system embodiments, wherein the system, specifically the scanning microscope system, is configured to extract Li conductive elements from a lithium bulk sample via the charged particle beam.

[0177] S38. The system according to any one of the foregoing two embodiments, wherein the system, specifically the scanning microscope system, is configured to extract the LTO conductive element from the lithium titanate bulk sample via the charged particle beam.

[0178] S39. A system according to any one of the foregoing system embodiments and having the features of embodiment S20, wherein the substrate includes a sample holder.

[0179] S40. The system according to the previous embodiment, wherein the sample holder includes an SEM sample holder.

[0180] S41. The system according to any one of the preceding two embodiments, wherein the sample holder comprises a plurality of arms, such as two arms, each of the plurality of arms being configured to provide conductive contact to at least one of the conductive elements.

[0181] S42. The system according to the previous embodiment, wherein each of the plurality of arms is connected to a voltage source such that a non-zero potential difference can be generated between any two of the plurality of arms.

[0182] S43. A system according to any of the foregoing system embodiments and having the features of embodiments S20 and S27, wherein the system is configured to transfer any conductive element of the conductive element onto the substrate (e.g., a sample holder) by means of a needle, wherein the needle comprises a microneedle.

[0183] S44. A system according to the preceding embodiment and having the features of embodiment S41, wherein transferring any of the plurality of conductive elements onto the substrate comprises transferring any conductive element onto any of the plurality of arms of the sample holder.

[0184] S45. A system according to the preceding embodiment and having the features of embodiment S20, wherein the step of transferring the at least one fluid onto the substrate precedes the step of transferring any of the plurality of conductive elements onto the substrate.

[0185] S46. A system according to any of the foregoing system embodiments and having the features of embodiment S34, wherein the result of the interaction between the charged particle beam and the at least one fluid includes transferring the fluid or a portion thereof to a region on the substrate, wherein the region corresponds to the gap between the at least two conductive elements.

[0186] S47. The system according to any one of the foregoing system embodiments, wherein the system is further configured to monitor the flow of the at least one fluid in response to the charged particle beam being directed onto the at least one fluid.

[0187] S48. The system according to any one of the foregoing system embodiments, wherein the system is configured to apply a non-zero voltage potential difference between the anode and the cathode and to measure the current between the anode and the cathode.

[0188] S49. The system according to the previous embodiment, wherein the system is further configured to stop the flow of the at least one fluid between the two conductive elements once a non-zero current is measured between the anode and the cathode.

[0189] S50. A system according to any one of the foregoing three embodiments and having the features of embodiment S47, wherein monitoring the flow of the at least one fluid further includes imaging the sample.

[0190] S51. A system according to the preceding embodiment and having the features of embodiment S33, wherein the system, specifically the scanning microscope system, is further configured to image the sample by detecting emission generated by the interaction between the charged particle beam and the at least one fluid.

[0191] S52. The system according to the previous embodiment, wherein the emission comprises photons.

[0192] S53. The system according to any one of the foregoing two embodiments, wherein the emission comprises electrons.

[0193] S54. The system according to the previous embodiment, wherein the electron includes any one of backscattered electrons, transmitted electrons, secondary electrons, or Auger electrons.

[0194] S55. The system according to any one of the foregoing four embodiments, wherein the emission comprises secondary ions.

[0195] S56. A system according to any one of the foregoing system embodiments and having the features of embodiment S51, wherein the image includes an SEM image.

[0196] S57. A system according to any of the foregoing system embodiments and having the features of embodiment S51, wherein the image includes a TEM image.

[0197] S58. A system according to any one of the foregoing system embodiments and having the features of embodiment S51, wherein the image includes a FIB image.

[0198] S59. A system according to any one of the foregoing system embodiments and having the features of embodiment S51, wherein the system, specifically the data processing system, includes a data storage element, and wherein the system is configured to store an image of the sample in the data storage element.

[0199] S60. The system according to the preceding embodiment, wherein the system further includes a display, and wherein the system is configured to display the sample image on the display.

[0200] S61. The system according to the preceding embodiment, wherein the system, specifically the data processing system, is configured to allow monitoring of the flow of the at least one fluid based on the displayed image.

[0201] S62. A system according to any one of the foregoing system embodiments and having the features of embodiments S23 and S24, wherein the system, specifically the data processing system, is configured to control the scanning position of the charged particle beam in a coordinate system associated with the sample by controlling the direction of the charged particle beam.

[0202] S63. A system according to any one of the foregoing system embodiments and having the features of embodiment S2, wherein the system, specifically the scanning microscope system, includes an electro-optic system configured to guide and / or focus the charged particle beam.

[0203] S64. The system according to the foregoing two embodiments, wherein the system, specifically the data processing system, is further configured to control the electro-optic system, and wherein the data processing system is configured to control the direction of the charged particle beam by controlling the electro-optic system.

[0204] S65. The system according to any one of the foregoing three embodiments, wherein the scanning microscope system comprises at least two or more electro-optic lenses.

[0205] S66. The system according to the previous embodiment, wherein the electro-optic lens includes at least one condenser lens and at least one objective lens.

[0206] S67. The system according to any one of the foregoing system embodiments, wherein processing the sample includes deposition and / or ablation of the sample or a portion thereof.

[0207] The following will discuss embodiments of the computer program product.

[0208] P1. A computer program product comprising instructions that, when run on a data processing system of the system according to any one of the foregoing system embodiments, are used to perform the method according to any one of the foregoing method embodiments.

[0209] Exemplary features of the present invention are further described in detail in the accompanying drawings and the following description of the drawings. Attached Figure Description

[0210] Figure 1 A scanning microscope system is shown.

[0211] Figure 2 The conductive element and the bulk material are shown.

[0212] Figure 3 The sample holder, two conductive elements, and ionic liquid are shown.

[0213] Figure 4 An embodiment of the method is shown.

[0214] Figure 5 A system configured to perform the method is shown. Detailed Implementation

[0215] For clarity, some figures may show only certain features while others may be omitted. However, omitted features are also possible, and the features depicted and discussed need not be present in all embodiments.

[0216] Figure 1 Components of a scanning microscope system 100 are shown. The scanning microscope system 100 can be configured to generate a main beam 107 of charged particles (e.g., electrons or ions). The scanning microscope system 100 can be further configured to guide the main beam 107 of charged particles onto a sample 108. The scanning microscope system 100 may include, for example, a focused ion beam (FIB) microscope or a scanning electron microscope (SEM) 101. In this example, the main beam comprises an ion beam. The charged particle beam may be generated by a charged particle source 102 configured to emit the charged particle beam, wherein a voltage may be applied between the charged particle source 102 and an extraction electrode 103. The applied voltage may preferably be in the range of at least 0.1 kV to at most 30 kV. In the case where the charged particle beam comprises ions, the source 102 may correspond to an ion source, and the extraction electrode 103 may correspond to a cathode. The scanning microscope system 100 may further include a orientation and / or focusing assembly, which may include, for example, an electromagnetic or electrostatic lens. Lenses can be configured to control the path of the main beam 107 (ion or electron beam). At least one condenser lens 104 can be included in an electromagnetic or electrostatic lens. The condenser lens 104 can be configured to control the size of the main beam 107. Furthermore, at least one objective lens 106 can be included in an electromagnetic lens. The objective lens 106 can be configured to focus the main beam 107 onto a scanning point on the sample 108. Depending on the particles comprising the charged particle beam, the scanning point can correspond to an ion or electron point on the sample 108. Further, the size and shape of the scanning point can depend on the focusing properties of the electromagnetic or electrostatic lens (e.g., the applied current) and the working distance between the FIB microscope 101 and the sample 108. Scanning coils or deflection electrodes 105 can be configured to deflect the main beam 107 across multiple scanning positions in one or two dimensions. Thus, optionally advantageously, this can achieve two-dimensional scanning of the sample.

[0217] The scanning microscope system 100 can be configured to detect first and second emissions 109, 111, 113. The main beam 107 can interact with particles (such as atoms) of the sample 108. This interaction can produce first and second emissions. The first emission can include the emission of charged particles, such as secondary electrons and / or secondary ions. The first emission can also include backscattered, transmitted, and / or Auger electron emissions. Furthermore, the second emission can include photon emissions across a wavelength range, such as X-rays and / or light (e.g., visible light).

[0218] exist Figure 1 In one example, the scanning microscope system 100 may include a first detector 110, which may be configured to sequentially detect backscattered electrons 109 emitted from a scanning position. Therefore, the first detector 110 may include a backscattered electron detector, such as a segmented silicon drift detector. However, a backscattered electron detector may also correspond to other types of solid-state detectors. Furthermore, the scanning microscope system 100 may include a second detector 112, which may be configured to sequentially detect secondary electrons and / or secondary ions 111 emitted from a scanning position. Therefore, the second detector may include a secondary electron detector, such as an Everhart-Thornley detector. The second detector may alternatively or additionally include a secondary ion detector, such as a charged particle multiplier.

[0219] Furthermore, the scanning microscope system may include a third detector 114, which may be configured to sequentially detect photons emitted from a scanning position. Therefore, the third detector 114 may include, for example, an X-ray detector, which may include, for example, a silicon drift detector. However, the third detector 114 may also include other types of photon detectors (e.g., photomultipliers or multi-pixel photon counters). The second detector 112 and the third detector 114 may be tilted relative to the surface of the sample 108.

[0220] The third detector 114 may be included in an energy-dispersive spectrometer (EDS). The energy bandwidth of the EDS may be in the range of 0 to at most 17 keV. In another form, the third detector 114 may be included in a wavelength-dispersive spectrometer (WDS). Furthermore, the third detector 114 may also be included in an electron energy loss spectrometer or a cathodoluminescence spectrometer.

[0221] Sample 108 can be positioned on top of movable platform 115. Movable platform 115 can be configured to perform two horizontal movements, a vertical movement, a tilting movement, and / or a rotational movement relative to the plane of sample 108. The two horizontal movements can include selecting the field of view. The vertical movement can include changing the height of sample 108, and thus changing the working distance and possible image resolution.

[0222] The scanning microscope system 100 may further include a control unit 116. The control unit 116 may be configured to control the power supply and operation of the condenser lens 104, objective lens 106, scanning coil or electrode 105, and movable platform 115. Furthermore, the scanning microscope system 100 may include a vacuum system. The vacuum system may include a vacuum controller 117, a mechanical pumping system 118, a (ultra)high vacuum pump 119 (such as an ion pump or turbomolecular pump), and a vacuum chamber 120. The vacuum controller 117 may be configured to control the operation of the mechanical pumping system 118 and the ultra-high vacuum pump 119. The mechanical pumping system 118 and the (ultra)high vacuum pump 119 may be configured to provide an (ultra)high vacuum within the vacuum chamber 120. The vacuum chamber 120 may be configured to contain a sample 108, the movable platform 115, a first detector 110 or a portion thereof, a second detector 112 or a portion thereof, a third detector 114 or a portion thereof, and a FIB or SEM microscope 101 or a portion thereof.

[0223] Figure 2 A conductive element 200 and a bulk material 201 are shown. The conductive element may correspond to an electrode, such as a lithium (Li) electrode, which can be extracted from the lithium bulk material. The conductive element may further correspond to a lithium titanate (LTO) electrode, which can be extracted from the lithium titanate bulk material. As will be understood by those skilled in the art, the electrode may include any other material extracted from the corresponding bulk material used in the battery system.

[0224] Figure 3 A liquid 300 and a sample holder 301 are shown, wherein the sample holder may include two arms. However, the arms may be independent of the sample holder. For example, an electrode may be held on a microneedle, wherein the needle may be connected to a circuit. Figure 3In this example, each arm can be configured to provide conductive contact to at least one of the conductive elements 200. The sample holder 301 can be included in a substrate such as a MEMS chip. Furthermore, a conductive element 200 (e.g., a lithium electrode) can be placed on each of the two arms of the sample holder. For example, a lithium electrode can be placed on one arm of the sample holder 301, and a lithium titanate electrode can be placed on the other arm of the sample holder 301. Liquid 300 may include organic cations such as 1-ethyl-3-methylimidazolium (EMIM), 1-butyl-3-methylimidazolium (BMIM), 1-octyl-3-methylimidazolium (OMIM), 1-decyl-3-methylimidazolium (DMIM), 1-butyl-2,3-dimethylimidazolium (DBMIM), 1-butyl-2,3-dimethylimidazolium (BMMIM), N-butyl-N-methylpyrrolidone (PYR14), N-methyl-N-propylpyrrolidone (PMPyr), N-methyl-N-propylpiperidinium (PP13), N-methyl-N-propylpyrrolidone (PYR13), or other organic cations. Liquid 300 may be an ionic conductor. Liquid 300 can move toward the conductive elements 200 on the sample holder 301, and specifically toward the area between the two conductive elements 200. The process of transferring liquid 300 is as follows: Figure 3 The right side is shown, in which liquid 300 is located between and partially on top of the conductive elements 200, thereby connecting the conductive elements.

[0225] Figure 4 An exemplary flowchart of a method according to an embodiment of the present invention is shown. A system may be configured to execute the method.

[0226] Figure 4 The method described herein may include three steps: a lifting step S1, a transfer step S2, and a forming step S3.

[0227] In the first step S1, which may be referred to as the extraction step, multiple conductive elements 200, such as two conductive elements 200, can be formed and extracted from multiple corresponding block samples (e.g., two corresponding block samples). For example, a lithium electrode can be extracted from a lithium block sample, and a lithium titanate electrode can be extracted from a lithium titanate block sample (as described above). Figure 4 In this example, each of the two conductive elements 200 is depicted by a small black box. The lift-off step may include milling (e.g., etching) a region of the corresponding bulk material using an ion beam. Specifically, the ion beam may interact with the bulk sample and sputter atoms from its surface. A portion of the bulk sample can thus be etched away to form a conductive element 200 of a specific size. This is also depicted in Figure 2The etching depth can depend on the energy of the ion beam and the total ion dose used for etching. The dose can be proportional to the ion beam current and etching time.

[0228] The second step S2, which may be referred to as the transfer step, may include removing and depositing conductive elements 200 on both arms of the sample holder 301. This step can be automated and can be performed, for example, by a microneedle. The transfer step S2 may further include depositing liquid 300 onto the substrate and close to the sample holder 301 using a pipette. In fact, the liquid can be placed at a distance of about 1 mm from the sample. When deposition is performed under an optical microscope and with a thin pipette fixed in the holder, this distance can be less than about 100 µm. Furthermore, the step of transferring liquid 300 onto the substrate may precede the step of transferring the two conductive elements 200 onto the substrate.

[0229] The third step S3, which may be referred to as the shaping step, may include moving and shaping the liquid 300 by means of an ion beam. Specifically, the method may include scanning an area of ​​the liquid 300 with an ion beam. The scanned area may correspond to an area of ​​the sample being imaged. In fact, the method may include recording an image of the sample while shaping the liquid. These images may be SEM images or FIB images. The shaping step may include scanning the liquid across the entire imaging area based on a recorded image and thus shaping the liquid. However, the shaping step may also include performing multiple scans on a smaller portion of the imaging area. Scanning the liquid 300 with the beam generates interactions between ions or electrons in the beam and ions in the liquid 300. These interactions may include thermal and / or electromagnetic interactions. Specifically, irradiating the liquid 300 with the beam may increase the temperature of the liquid 300, whereby the increased temperature may subsequently reduce the viscosity of the liquid. Therefore, due to the reduced friction between the liquid 300 and the substrate, the liquid 300 can be easily guided and transferred to the desired location. The result of connecting two conductive elements 200 through the liquid 300 can enable the fabrication of microstructures capable of conducting ions. Figure 4 In examples, the conductive microstructure can include a cell 500, such as a microcell. The size of a microcell 500 is typically in the tens of micrometers. Specifically, the cell size can range from 0.1 µm to a few hundred micrometers (at most about 200-300 µm). However, the fabricated cell 500 can also be much larger than the aforementioned size. The described process can be used with a bulk material used as one electrode (not fabricated by FIB, but simply a bulk formation, e.g., one of the arms; in size from centimeters to tens of centimeters), and a second electrode can be placed next to said first electrode using FIB and liquid (the last two according to...). Figure 4The battery may specifically include a Li-EMIM-LTO battery. The method may further include stopping the flow of liquid 300 between the two conductive elements 200 once they are connected by liquid 300, which can be observed using FIB or SEM imaging or measured in a circuit containing the conductive elements 200. For example, such a circuit may include a non-zero potential difference generated between the two arms of a sample holder 301, on which the conductive elements 200 may be placed. The potential difference may be within a chamber that can accommodate the sample holder 301 (e.g., Figure 1 The vacuum chamber 120 of the scanning microscope system 100 depicted is generated outside. The net current flowing through such a circuit can then indicate successful contact between the liquid 300 and the two conductive elements 200.

[0230] Figure 5 The system is illustrated. The system can be configured to perform the methods described above.

[0231] The system includes a scanning microscope system 100 and a data processing system 600.

[0232] Data processing system 600 may include one or more processing units configured to implement computer instructions (i.e., machine-readable and executable instructions). The processing units may be single or multiple. For example, data processing system 600 may include at least one of a CPU, GPU, DSP, APU, ASIC, ASIP, or FPGA.

[0233] The data processing system 600 may include a memory component, such as a data storage component 610. The data storage component 610 and the data processing system 600 may include at least one of main memory (e.g., RAM), cache memory (e.g., SRAM), and / or secondary memory (e.g., HDD, SDD).

[0234] The data processing system 600 may include volatile and / or non-volatile memory, such as SDRAM, DRAM, SRAM, flash memory, MRAM, F-RAM, or P-RAM. The data processing system 600 may include an internal communication interface (e.g., a bus) configured to facilitate electronic data exchange between components of the data processing system 600, such as communication between memory components and processing components.

[0235] The data processing system 600 may include an external communication interface configured to facilitate electronic data exchange between the data processing system 600 and external devices or networks. Figure 5In this example, the external communication interface can be configured to facilitate electronic connection between the processing components of the data processing system 600 and components of the scanning microscope system 100 (such as the control unit 116). Furthermore, the external communication interface can be configured to establish electronic data exchange between the processing components of the data processing system 600 and the vacuum controller 117.

[0236] Furthermore, the external communication interface can also be configured to establish electronic data exchange between the data processing system 600 and the first, second, and third detectors (110, 112, 114). For example, detected secondary electronic data from each scan position can be stored in the data storage component 610. The processing unit of the data processing system 600 can be configured to form at least one image based on the stored secondary electronic data.

[0237] The secondary electronic image of the sample can be stored in the data storage component 610.

[0238] The data processing system 600 may also include a network interface card, which can be configured to connect the data processing system 600 to a network, such as the Internet. The data processing system 600 can be configured to use standardized communication protocols to transmit electronic data. The data processing system 600 can be a centralized or distributed computing system.

[0239] The data processing system 600 may include a user interface, such as an output user interface and / or an input user interface. For example, an output user interface may include a screen and / or monitor configured to display visual data (e.g., a secondary electron image or X-ray spectrum of a sample) or a speaker configured to transmit audio data (e.g., play audio data to a user). An input user interface may include, for example, a keyboard and / or touchpad, mouse, touchscreen, and / or joystick configured to allow the insertion of text and / or other keyboard commands (e.g., allowing the user to input instructions or parameters of a scanning microscope system or method), which may be configured, for example, to navigate a secondary electron image or identify an area within the secondary electron image.

[0240] In simple terms, data processing system 600 can be a processing unit configured to execute program instructions. Data processing system 600 can be a system-on-a-chip including a processing unit, memory components, and a bus. Data processing system 600 can be a personal computer, laptop computer, pocket computer, smartphone, or tablet computer. Data processing system 600 can include a server, a server system, a part of a cloud computing system, or a system simulating a server, such as a server system with appropriate software for running virtual machines. Data processing system 600 can be a processing unit or a system-on-a-chip that can be connected to a personal computer, laptop computer, pocket computer, smartphone, tablet computer, and / or a user interface (such as the user interface mentioned above).

[0241] While preferred embodiments have been described above with reference to the accompanying drawings, those skilled in the art will understand that these embodiments are provided for illustrative purposes only and should not in any way be construed as limiting the scope of the invention, which is defined by the claims.

[0242] Whenever relative terms such as “about,” “substantially,” or “approximately” are used in this specification, such terms should also be interpreted as including exact terms. That is, for example, “substantially straight” should be interpreted as including “(exactly) straight.”

[0243] Whenever a step is recited in the foregoing or appended claims, it should be noted that the order in which the steps are recited herein may be accidental. That is, unless otherwise stated or unless it is clear to a person skilled in the art, the order in which the steps are recited may be accidental. That is, when this document states, for example, that a method includes steps (A) and (B), this does not necessarily mean that step (A) precedes step (B), but it is also possible that step (A) is performed (at least partially) concurrently with step (B), or that step (B) precedes step (A). Furthermore, when it is said that step (X) precedes another step (Z), this does not mean that there are no steps between steps (X) and (Z). That is, step (X) preceding step (Z) covers the case where step (X) is performed directly before step (Z), and also covers the case where (X) is performed before one or more steps (Y1)... followed by step (Z). Corresponding considerations apply when using terms such as "after" or "before".

[0244] Figure Labels 100 Scanning Microscope System 101. Focused ion beam microscope or scanning electron microscope 102 Charged Particle Source 103 Lead-out electrode 104 Condensing Lens 105 Scanning coil or scanning electrode 106 Objective Lenses 107 main beams of charged particles 108 samples 109 Emission of backscattered electrons 110 First Detector 111 Emission of secondary electrons and / or secondary ions 112 Second Detector 113 X-ray photon emission 114 Third Detector 115 Mobile Platform 116 Control Unit 117 Vacuum Controller 118 Mechanical pumping system 119 (Ultra) High Vacuum Pump 120 Vacuum Chamber 200 Conductive Element 201 Block Material 300 Ionic Liquid 301 Sample Holder S1 Lifting Step S2 Transfer Steps S3 Forming Step 500 microcells 600 Data Processing System 610 Data storage component.

Claims

1. A method for preparing and / or processing a sample, wherein: The sample includes at least one fluid and multiple conductive elements; and The method includes: Directing a charged particle beam onto the at least one fluid and causing the at least one fluid to flow in response to the charged particle beam being directed onto the at least one fluid; and Perform a lift-out step, wherein the lift-out step includes milling and removing the plurality of conductive elements from the plurality of corresponding block samples.

2. The method of claim 1, wherein the at least one fluid comprises an electrical conductor, and the at least one fluid comprises an ionic liquid.

3. The method of claim 1, wherein the plurality of conductive elements comprise electrodes, such that one conductive element comprises an anode and another conductive element comprises a cathode.

4. The method of claim 1, wherein the method further comprises a transfer step, wherein the sample comprises a substrate, and wherein the transfer step comprises transferring any of the plurality of conductive elements onto the substrate.

5. The method of claim 4, wherein the substrate includes a sample holder comprising a plurality of arms, each of the plurality of arms being configured to provide conductive contact to at least one of the plurality of conductive elements, and wherein the transfer step further comprises transferring any conductive element to any arm of the plurality of arms of the sample holder, and wherein the method further comprises monitoring the flow of the at least one fluid in response to the charged particle beam being directed onto the at least one fluid, wherein monitoring the flow of the at least one fluid further comprises connecting each of the plurality of arms to a voltage source such that a non-zero potential difference can be generated between any two arms of the plurality of arms, and stopping the flow of the at least one fluid between the two conductive elements once a non-zero current is measured between the anode and cathode of the plurality of conductive elements.

6. The method of claim 3, wherein the plurality of conductive elements are positioned at a distance greater than 1 nm from each other, and wherein the flow of at least one fluid in response to the guided charged particle beam comprises transferring at least a portion of the fluid to a region of the sample, wherein the region corresponds to the gap between the conductive elements.

7. The method of claim 1, wherein the method further comprises monitoring the flow of the at least one fluid in response to the charged particle beam being directed onto the at least one fluid, wherein monitoring the flow of the at least one fluid further comprises imaging the sample.

8. A system comprising a scanning microscope system and a data processing system, wherein the system is configured to prepare and / or process a sample, wherein the sample comprises at least one fluid and a plurality of conductive elements, and wherein the system is configured to: Directing a charged particle beam onto the at least one fluid and causing the at least one fluid to flow in response to the charged particle beam being directed onto the at least one fluid; and Perform a lift-out step, wherein the lift-out step includes milling and removing the plurality of conductive elements from the plurality of corresponding block samples.

9. The system of claim 8, wherein the scanning microscope system includes an electro-optic system configured to guide and / or focus the charged particle beam, and wherein the data processing system is further configured to control the electro-optic system, and wherein the data processing system is configured to control the direction and / or focus of the charged particle beam by controlling the electro-optic system.

10. The system of claim 9, wherein the scanning microscope system is configured to scan the charged particle beam across the at least one fluid at multiple scanning positions in one, two, or three dimensions, and wherein the result of scanning the charged particle beam across the at least one fluid at the scanning positions includes the interaction between the charged particle beam and the at least one fluid.

11. The system of claim 10, wherein the scanning microscope system is further configured to image the sample by detecting emission generated by the interaction of the charged particle beam with the at least one fluid, and wherein the system is configured to display an image of the sample on a display and allow monitoring of the flow of the at least one fluid based on the displayed image.

12. A memory component storing instructions that, when executed by a processor, cause the processor to perform the method according to any one of claims 1-7.

13. A computer program product comprising instructions that, when executed by a processor, cause the processor to perform the method according to any one of claims 1-7.

Citation Information

Patent Citations

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    CN111646425A