Systems and methods for performing sample extraction on highly reactive materials

Abstract

Methods and systems are disclosed herein for creating an attachment between a sample manipulator and a sample within a charged particle system. The method includes translating the sample manipulator so that it is close to the sample and milling a portion of the sample manipulator so that a portion is removed. The portion of the sample manipulator close to the sample is made of a high sputtering yield material, and the high sputtering yield material can be a material milled using a charged particle beam so that it is removed from the sample manipulator. According to the present disclosure, the portion of the sample manipulator is milled so that at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample.

Description

BACKGROUND OF THE INVENTION

[0001] In a scanning and transmission charged particle microscope, a charged particle beam is used to image or otherwise study a region of interest on a sample. In many situations, it is often necessary to prepare and / or manipulate the sample within the system to allow exposure or otherwise prepare the region of interest before the region of interest can be imaged and / or studied. In current systems, such preparation typically involves one or more of the following: preparing a sample from a larger specimen using a charged particle beam, attaching the sample to a manipulation probe to allow translation of the sample within the microscope system, and attaching the sample to a sample holder such that the region of interest on the sample can be processed, imaged, and / or otherwise studied.

[0002] In current systems, the sample is attached to the probe and / or sample holder using a precursor gas or a deposition liquid. Specifically, in some attachment methods, a precursor gas is introduced into the volume surrounding the sample, where gas molecules form deposits on the sample, the probe, and / or the sample holder when irradiated by the charged particle beam. In another current attachment method, a liquid is first introduced to the sample, the probe, and / or the sample holder, and the liquid is irradiated using the charged particle beam such that it is cured, thereby forming an attachment bond between the sample and the probe and / or the sample holder. However, while these systems are suitable for many general applications, they each have drawbacks that make them unsuitable for some microscopy studies.

[0003] For example, a charged particle microscope system studies a sample in a sealed chamber to reduce contamination of optical components, reduce the effect of unwanted particles on the charged particle beam, and have no unwanted deposits on the sample. The introduction of a precursor gas and / or liquid adds additional material to the chamber of the charged particle microscope system, increasing these unwanted effects. Additionally, the introduction of a gas or liquid requires a specially customized mechanism, which complicates the design and implementation of new charged particle systems while also adding complex processing steps that are difficult for new users to accurately implement. Finally, for highly reactive samples, traditional precursor gases cannot be used because the introduction of the gas may cause degradation of the sample surface and / or cause the sample to be more reactive to the charged particle beam during subsequent attachment milling or imaging. As such, there is a need for new attachment and sample manipulation systems and processes to allow imaging and study of highly reactive materials. SUMMARY OF THE INVENTION

[0004] Methods and systems are disclosed herein for creating an attachment between a sample manipulator and a sample within a charged particle system. The method includes translating the sample manipulator so that it is close to the sample, and milling a portion of the sample manipulator so that a portion is removed. The portion of the sample manipulator that is close to the sample is made of a high sputter yield material, and the high sputter yield material can be a material that is milled using a charged particle beam so that it is removed from the sample manipulator. According to the present disclosure, the portion of the sample manipulator is milled so that at least some of the high sputter yield material that is removed is redeposited to form an attachment between the sample manipulator and the sample.

[0005] A system for creating an attachment between a sample manipulator and a sample within a charged particle system according to the present disclosure can include: a charged particle emitter configured to emit charged particles towards the sample; a sample holder configured to support the sample; an optical column configured to direct the charged particles to be incident on the sample; and a detector system configured to detect emissions from the sample due to charged particle irradiation. The system further includes one or more processors and a memory storing non-transitory computer-readable instructions that, when executed by the one or more processors, cause the microscope system to translate the sample manipulator so that it is close to the sample, and mill the high sputter yield portion of the sample manipulator so that the material removed by milling is redeposited to form an attachment between the sample manipulator and the sample. Description of the Drawings

[0006] The detailed description is described with reference to the accompanying drawings. In the drawings, the leftmost digit of the reference numeral identifies the drawing in which the reference numeral first appears. The same reference numerals in different drawings indicate similar or identical items.

[0007] Figure 1 An example system is illustrated for performing sample extraction and protection cap placement for highly reactive materials and / or for creating an attachment between a sample manipulator and a sample within a charged particle microscope system.

[0008] Figure 2 A flowchart of an illustrative process for performing sample extraction and protection cap placement for highly reactive materials within a charged particle microscope system.

[0009] Figure 3 A series of captured images that show an example execution for performing sample extraction and protection cap placement for highly reactive materials within a charged particle microscope system.

[0010] Figures 4A to 4C A captured image that shows an example result of sample extraction and protection cap placement for highly reactive materials according to the present disclosure.

[0011] Figure 5 A flowchart depicting an illustrative process for creating an attachment between a sample manipulator and a sample within a charged particle system.

[0012] Figures 6A to 6C An example embodiment for creating an attachment between a sample manipulator and a sample within a charged particle system is shown.

[0013] Figure 7 A series of images are shown that depict an example execution of an example process for sample extraction and protection cap placement for highly reactive materials using a sample holder with beveled edges.

[0014] Throughout several views of the drawings, like reference numerals refer to corresponding parts. DETAILED DESCRIPTION

[0015] Methods and systems for performing sample extraction and protection cap placement for highly reactive materials within a charged particle microscope system are disclosed. More specifically, the present disclosure includes methods and systems in which: a nested void is created in a support structure, the sample is translated such that at least a portion of the sample is located within the nested void, and then material from the region of the support structure that defines the nested void is milled away. The material from the region of the support structure is located near the sample such that at least some of the removed material is redeposited to form one or more attachment bonds between the sample and the remainder of the support structure. In this way, the sample can be attached to a sample holder without the need to add a precursor gas or other type of attachment medium to the charged particle system. Additionally, because the attachment is formed by passive redeposition of the milled material, there is much less chance of reacting and / or otherwise damaging the sample. This allows samples composed of highly reactive materials (e.g., samples found in lithium-based battery technologies) to be attached to a sample holder without damaging the sample. Once the sample is attached to the sample holder in this manner, one or more methods can be used to image and / or study one or more regions of interest of the sample, such as but not limited to serial section tomography of the sample, enhanced insertable backscattered detector (CBS) analysis of the sample, and electron backscatter diffraction (EBSD) analysis of the sample.

[0016] In addition, methods and systems for creating an attachment between a sample manipulator and a sample within a charged particle system are also disclosed herein. Specifically, the present disclosure includes the following methods and systems, wherein: the sample is attached to a holder or manipulator by irradiation of a high sputtering yield material near the sample. Initially, the sample manipulator is translated so that a portion of the manipulator made of a high sputtering yield material is located near the sample (e.g., within one micron). Next, a charged particle beam is used to mill away an area of ​​high sputtering yield material near the sample, so that at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample. According to the present disclosure, when irradiated with a specific ion beam material and voltage other than silicon or tungsten, the high sputtering yield material corresponds to a material that produces a large number of atoms per ion. For example, when a 30 kV Ga+ focused ion beam such as copper or zinc is used to irradiate the material, the high sputtering yield material is a high sputtering yield material defined as a material that emits more than 5, 7, 8, or 10 atoms per ion.

[0017] Generally, in the drawings, elements that may be included in a given example are shown in solid lines, while elements that are optional for a given example are shown in dashed lines. However, elements shown in solid lines are not necessary for all examples of the present disclosure, and elements shown in solid lines may be omitted from a particular example without departing from the scope of the present disclosure.

[0018] Figure 1 An example system 100 is shown for performing sample extraction and protective cap placement for highly reactive materials and / or for creating an attachment between a sample manipulator and a sample within a charged particle microscope system. Specifically, Figure 1 An example environment 102 is shown that includes an example microscope system 104 for creating an attachment between a sample manipulator 106 and a sample 108 and / or performing sample extraction and protective cap placement in situ for highly reactive materials. It should be noted that the present disclosure is not limited to environments that include microscopes, and in some embodiments, the environment 100 may include different types of systems configured to manipulate and / or otherwise examine the sample 108.

[0019] The example microscope system 104 may be or include one or more different types of optical and / or charged particle microscopes, such as, but not limited to, a scanning electron microscope (SEM), a scanning transmission electron microscope (STEM), a transmission electron microscope (TEM), a charged particle microscope (CPM), a cryo-compatible microscope, a focused ion beam (FIB) microscope, a dual beam microscope system, or a combination thereof. Figure 1 The example microscope system 104 is shown as a dual-beam microscope system including a STEM column 110 and a FIB column 112 .

[0020] Figure 1The exemplary microscope system 104 is depicted as including a STEM column 110 for irradiating a sample 108 with a charged particle beam 114. The SEM column 110 includes an electron source 116 (e.g., a thermionic source, a Schottky emission source, a field emission source, etc.), which emits an electron beam 114 along an electron emission axis 118 and toward the sample 108. The electron emission axis 118 is a central axis that extends along the length of the exemplary microscope system 104 from the electron source 116 and through the sample 108. Although Figure 1 the exemplary microscope system 104 is depicted as including an electron source 116, in other embodiments, the STEM column 110 may include a charged particle source, such as an ion source, configured to emit a plurality of charged particles toward the sample 108.

[0021] An accelerator lens 120 accelerates / decelerates, focuses, and / or directs the electron beam 114 to an electron focusing column 122. The electron focusing column 122 focuses the electron beam 114 such that it impinges on at least a portion of the sample 108. Additionally, the focusing column 122 may correct and / or tune aberrations (e.g., geometric aberrations, chromatic aberrations) of the electron beam 114. In some embodiments, the electron focusing column 122 may include one or more of pores, deflectors, transfer lenses, scanning coils, condenser lenses, objective lenses, etc., which together focus electrons from the electron source 116 onto a small spot on the sample 108. Different positions of the sample 108 may be scanned by adjusting the direction of the electron beam via a deflector and / or a scanning coil. In this manner, the electron beam 114 may act as an imaging beam that scans across a surface layer of the sample (i.e., a surface of a layer near the STEM column 104 and / or irradiated by the electron beam 114). This irradiation of the surface layer of the sample 108 causes the constituent electrons of the electron beam 114 to interact with the constituent elements / molecules / features of the sample, such that the constituent elements / molecules / features cause an emission 124 to be emitted by the sample 108. The particular emission released is based on the corresponding element / molecule / feature that caused it to be emitted, such that the emission can be analyzed to determine information about the corresponding element / molecule. Additionally, although Figure 1 the emission 124 is depicted as traveling downstream of the sample 108, those skilled in the art will understand that the emission may be released in other directions, including but not limited to toward the charged particle source 116.

[0022] Figure 1Further illustrated are detector systems 126(a) and 126(b) for detecting emissions 124 incident on sample 108 generated from electron beam 114. The detector system 126 may include one or more detectors positioned or otherwise configured to detect such emissions. For example, a charged particle system according to the present invention may include detector system 126(a) positioned below sample 108, detector system 126(b) positioned above sample 108, or both. In various embodiments, different detectors and / or different portions of a single detector may be configured to detect different types of emissions, or configured such that parameters of emissions detected by different detectors and / or different portions are different. The detector system 126 is further configured to generate data / data signals corresponding to the detected emissions and transmit the data / data signals to one or more computing devices 128.

[0023] Meanwhile Figure 1 The exemplary microscope system 104 is also depicted as including an FIB column 112 for removing portions of sample 108 or other objects in microscope chamber 130. For example, the FIB column 112 may be used to mill away portions of the sample body to expose or otherwise create sample 108. In other embodiments, the exemplary microscope system 104 may include other types of delamination components, such as lasers, mechanical blades (e.g., diamond blades), electron beams, etc. The FIB column 112 is shown as including a charged particle emitter 132 configured to emit a plurality of ions 134 along an ion emission axis 136.

[0024] The ion emission axis 136 is a central axis extending from the charged particle emitter 132 and passing through the center of sample 108. The FIB column 112 further includes an ion focusing column 138 that includes one or more of pores, deflectors, transfer lenses, scan coils, condenser lenses, objective lenses, etc., which together focus the ions from the charged particle emitter 132 onto a small spot on sample 108. In this way, the elements in the ion focusing column 138 may mill away or otherwise remove one or more portions of sample 108 or other body. For example, during sectioning and view imaging, the FIB column 112 may be configured such that a surface layer of sample 108 having a known thickness is removed from sample 108 between image acquisitions.

[0025] Figure 1The exemplary microscope system 104 is further illustrated as further including a sample holder 140, a sample manipulator 106, and a sample loading chamber 142. The sample holder 140 is configured to hold the sample 108 and the sample 108 can be translated, rotated, and / or tilted relative to the exemplary microscope system 104. For example, the sample holder 140 may include a grid or structure to which the sample or specimen will be attached and / or otherwise held. Additionally, the sample manipulator 108 is a mechanism within the microscope chamber 130 that is capable of interacting with the sample 108 such that the sample can be translated, tilted, and / or rotated. For example, Figure 1 the sample manipulator is shown as including a probe portion that extends from a body and to which the sample can be attached. The sample loading chamber 142 may be isolatable from the microscope chamber 130 and may allow the sample holder 140 to be retracted therein such that a user may be able to access and / or interact with the sample holder 140 while the sample holder is within the sample loading chamber 142.

[0026] The environment 100 is also shown as including one or more computing devices 128. Those skilled in the art will appreciate that, Figure 1 the computing devices 128 depicted are merely illustrative and are not intended to limit the scope of the present disclosure. Computing systems and devices may include any combination of hardware or software that can perform the indicated functions, including computers, network devices, Internet devices, PDAs, wireless telephones, controllers, oscilloscopes, amplifiers, etc. The computing device 128 may also be connected to other devices not shown or, conversely, may operate as a stand-alone system.

[0027] It should also be noted that one or more of the computing devices 128 may be components of the exemplary microscope system 104, may be devices separate from the exemplary microscope system 104 that communicate with the exemplary microscope system 104 via a network communication interface, or a combination thereof. For example, the exemplary microscope system 104 may include a first computing device 128 that is an integral part of the exemplary microscope system 104 and that serves as a controller that drives the operation of the exemplary charged particle microscope system 104 (e.g., adjusts the scan position on the sample by operating scan coils, etc.). In such embodiments, the exemplary microscope system 104 may further include a second computing device 128 that is a desktop computer separate from the exemplary microscope system 104 and that may execute to process data received from the detector system 126 to generate an image of the sample 108 and / or perform other types of analysis or post-processing on the detector data. The computing device 128 may further be configured to receive user selections via a keyboard, mouse, touchpad, touchscreen, etc. The computing device 128 is configured to generate an image of the surface layer of the sample 108 within the exemplary microscope system 104 based on data and / or data signals from the detector system 126.

[0028] In addition, the computing device 128 is configured to control the FIB column 112, the sample manipulator 106, and / or the sample holder 140 to allow for sample extraction and protective cap placement for highly reactive materials within the charged particle microscope system 104. For example, the computing device 128 may cause the FIB column 112 to mill nested voids in a support structure (such as a sample grid, a sample holder, or other structure that allows imaging / study of the sample when attached thereto) using a plurality of ions 134. One or more user selections, automated procedures, or combinations thereof may allow the computing device 128 to cause the sample holder 140 or the sample manipulation device 106 to translate (e.g., translate, tilt, and / or rotate) such that at least a portion of the sample 108 is positioned within the nested voids. Once the sample 108 is at least partially positioned within the nested voids, the computing device 128 may cause the FIB column 112 to mill away the portion of the support structure adjacent to the sample and / or the portion defining the nest. A user selection, automated procedure, or combination thereof selects the portion of the support structure to be milled in this manner such that the milled material is redeposited to form an attachment bond between the support structure and the portion of the sample 108 within the nested voids. In this way, an interconnection is formed between the sample 108 and the support structure such that the sample 108 is held in place for further processing / imaging without the need to add deposition gas or other materials to the microscope chamber 130. In some embodiments, the computing device 128 may further be configured to cause the exemplary microscope system 104 to prepare the sample 108 (e.g., remove the sample from a larger sample body, expose the surface / structure of interest) prior to attachment, process the sample to ready it for imaging / survey, or perform imaging / survey of one or more regions of the sample 108.

[0029] Alternatively or additionally, the computing device 128 may be configured to create one or more attachments between the sample manipulator 106 and the sample 108 within the charged particle system 104 without adding additional deposition gas or other materials to the microscope chamber 130. For example, the computing device 128 may cause a high sputtering yield material (such as copper) to be positioned adjacent to the sample 108. The high sputtering yield material may optionally be attached to the sample manipulator, which itself may include a high sputtering yield material (e.g., comes with this coating when purchased, or has the coating added in situ or ex situ when purchased).

[0030] A user selection, an automated procedure, or a combination thereof may then cause the computing device 128 to activate the FIB column 112 to mill away portions of the high sputter yield material that are close to the sample, while leaving one or more other portions of the high sputter yield material that are located near the sample manipulator and that have not been milled. In this way, although some portions of the high sputter yield material that are close to the sample are removed, there are still portions of the material that are within 10 microns, 1 micron, or closer to the sample. Thus, when the milled high sputter yield material is redeposited, it forms one or more attachment bonds between the sample and the sample manipulator.

[0031] Figure 1 Further included is a schematic diagram illustrating an example computing architecture 150 of the computing device 128. The example computing architecture 150 illustrates additional details of the hardware and software components that can be used to implement the techniques described in this disclosure. Those skilled in the art will understand that the computing architecture 150 can be implemented in a single computing device 128 or can be implemented across multiple computing devices. For example, the individual modules and / or data constructs depicted in the computing architecture 150 can be executed by different computing devices 128 and / or stored on different computing devices 128. In this way, the different process steps of the inventive methods disclosed herein can be implemented and / or executed by separate computing devices 128 and in various orders within the scope of this disclosure. In other words, in some embodiments, the functionality provided by the illustrated components can be combined in fewer components or distributed across additional components. Similarly, in some embodiments, the functionality of some of the illustrated components may not be provided and / or other additional functionality may be used.

[0032] In the example computing architecture 150, the computing device includes one or more processors 152 and a memory 154 communicatively coupled to the one or more processors 152. Although not intended to be limiting, the example computing architecture 150 is shown as including a control module 156 stored in the memory 154. As used herein, the term "module" is intended to represent an instance partitioning of executable instructions for discussion purposes and is not intended to denote any type of requirement or required method, manner, or organization. Thus, although various "modules" are described, their functionality and / or similar functionality can be arranged differently (e.g., combined into a smaller number of modules, broken down into a large number of modules, etc.). Additionally, although specific functions and modules are described herein as being implemented by software and / or firmware executable on a processor, in other examples, any one or all of the modules can be implemented in whole or in part by hardware (e.g., a dedicated processing unit, etc.) to perform the described functions. As discussed above in various embodiments, the modules described herein in connection with the example computing architecture 150 can be executed across multiple computing devices 128.

[0033] The control module 156 can be executed by the processor 152 to cause the computing device 128 and / or the exemplary microscope system 104 to adopt one or more actions and / or perform the functions or maintenance of the system. In some embodiments, the control module 156 can cause the exemplary microscope system 204 to perform sample extraction and / or protective cap placement for highly reactive materials within the charged particle microscope system 104. For example, the control module 156 can cause the exemplary microscope system 204 to perform this process using the exemplary process described in the notes regarding Figure 2 to 4. Alternatively, or in addition, the control module 156 can be configured to cause the exemplary microscope system 204 to create one or more attachments between the sample manipulator 106 and the sample 108 within the charged particle system 104 without adding additional deposition gas or other materials to the microscope chamber 130. For example, the control module 156 can cause the exemplary microscope system 204 to perform this process using the exemplary process described in the notes regarding Figures 5 to 7 .

[0034] As discussed above, the computing device 128 includes one or more processors 152 that are configured to execute instructions, applications, or programs stored in a memory 154 accessible by the one or more processors. In some instances, the one or more processors 152 can include hardware processors that include, but are not limited to, a hardware central processing unit (CPU), a graphics processing unit (GPU), and the like. Although in many cases the techniques are described herein as being executed by one or more processors 152, in some cases the techniques can be implemented by one or more hardware logic components, such as a field programmable gate array (FPGA), a complex programmable logic device (CPLD), an application specific integrated circuit (ASIC), a system on a chip (SoC), or a combination thereof.

[0035] The memory 154 accessible to the one or more processors 152 is an example of a computer-readable medium. Computer-readable media can include two types of computer-readable media, namely computer storage media and communication media. Computer storage media can include volatile and non-volatile media and removable and non-removable media that implement information storage such as computer-readable instructions, data structures, program modules, or other data in any method or technology. Computer storage media includes, but is not limited to, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EEPROM), flash memory or other memory technologies, compact disc read-only memory (CD-ROM), digital versatile disks (DVD) or other optical storage devices, magnetic tape cassettes, magnetic tapes, magnetic disk storage devices or other magnetic storage devices, or any other non-transmission medium that can be used to store the required information and can be accessed by a computing device. Generally speaking, computer storage media can include computer-executable instructions that, when executed by one or more processing units, perform the various functions and / or operations described herein. In contrast, communication media embodies computer-readable instructions, data structures, program modules, or other data in a modulated data signal such as a carrier wave, or other transmission mechanism. As defined herein, computer storage media does not include communication media.

[0036] Those skilled in the art will also appreciate that, for purposes of memory management and data integrity, items or portions thereof may be transferred between the memory 154 and other storage devices. Alternatively, in other embodiments, some or all of the software components may be executed in the memory of another device and communicate with the computing device 128. Some or all of the system components or data structures may also be stored (e.g., as instructions or structured data) on a non-transitory computer-accessible medium or portable article for reading by an appropriate drive, various examples of which are described above. In some embodiments, instructions stored on a computer-accessible medium separate from the computing device 128 may be transmitted to the computing device 128 via a transmission medium or signal (such as an electrical, electromagnetic, or digital signal delivered via a communication medium such as a wireless link). Various embodiments may further include receiving, sending, or storing instructions and / or data implemented on a computer-accessible medium as described above.

[0037] Figure 2 and 5A flowchart of an illustrative process that is presented as a collection of blocks in a logical flowchart diagram, representing a series of operations that can be implemented in hardware, software, or a combination thereof. In the context of software, the blocks represent computer-executable instructions stored on one or more computer-readable storage media that perform the recited operations when executed by one or more processors. Generally, computer-executable instructions include routines, programs, objects, components, data structures, etc. that perform specific functions or implement specific abstract data types. The order of description of the operations is not intended to be construed as a limitation, and any number of the described blocks can be combined in any order and / or in parallel to implement the process.

[0038] Specifically, Figure 2 A flowchart of an illustrative process 200 for performing sample extraction and protective cap placement for highly reactive materials within a charged particle microscope system. Process 200 can be implemented in the example charged particle microscope setup 100 described above and / or by the computing architecture 150 or in other environments and architectures.

[0039] At 202, the sample is optionally prepared. For example, the sample can be pre-treated to expose the region of interest to be imaged and / or studied. In some embodiments, this can include using a process for forming a sample from a larger sample, such as a sample extraction procedure, where portions of the sample are milled away to expose a block containing the region of interest, the block is attached to a sample manipulator, the block is detached from the body of the sample, and the sample manipulator and / or the sample are translated such that the block is moved away from the sample body. Alternatively or additionally, the surface of the sample can be milled away and / or polished to expose the region of interest and / or remove damage from the surface to allow for high-quality imaging / study. In some embodiments, the sample can correspond to a battery or a part of a battery, and the sample can be a part thereof that includes at least one of lithium, manganese, lithium polymer, lithium cobalt oxide, lithium manganese oxide, lithium manganese cobalt oxide, etc.

[0040] At 204, a nested void is prepared in the support structure. Specifically, a nested void is prepared in the support structure by removing a volume of material from the support structure to create a volume in which at least a portion of the sample can be accommodated. For example, a charged particle beam can be used to mill away material from the support structure. The nested void can correspond to a hole, recess, or insertion volume into which a portion of the sample can be inserted. In some embodiments, the support structure can be a sample holder having beveled edges (e.g., 45-degree beveled edges), and the nested void can be a portion of the sample holder that is milled away using a focused ion beam near the beveled edges. The nested void can be milled such that at least a portion of the beveled holder extends beyond the sample when the sample is inserted into the nested void.

[0041] In various embodiments, the support structure can correspond to one or more of a sample grid, a sample holder, or other structures that allow imaging / studying of the sample when the sample is attached thereto. The support structure can be at least partially composed of many different materials, including but not limited to silicon, aluminum, copper, etc. In some embodiments, the support structure is composed of an inert material that is non-reactive to charged particle beams.

[0042] At 206, the sample is translated such that at least a portion of the sample is positioned within the nested void. For example, the sample can be attached to a movable sample manipulator (e.g., a sample probe) that is translated, tilted, and / or rotated such that at least a portion of the sample is received within the nested void. That is, the sample is positioned such that the portion of the sample is located within the volume in which the milled-away portion of the support structure is located.

[0043] At 208, a portion of the support structure is milled away. Specifically, the portion of the support structure that is proximate to the sample and / or that defines the nested void is milled away from the support structure. In some embodiments, the edges / surfaces of the support structure that define the nested void are milled away along the depth of the sample. Alternatively or additionally, multiple portions of the support structure that partially define the nested void can be milled away in this manner. For example, a charged particle beam can be used to mill away multiple different portions of the support structure, each portion of which partially defines the nested void along one or more surfaces of the nested void. Such multiple different portions of the support structure can be milled such that between the milled portions, protrusions of the support structure remain close to the sample.

[0044] At 210, the milled-away material is allowed to redeposit to form an attachment bond between the sample and the support structure. Although a portion of the support structure is milled away at step 208 and immediately thereafter, the sample is held in a constant position such that the milled-away material is allowed to settle on the non-milled portions of the support structure and / or the sample. In this manner, the milled-away material is allowed to form interconnects to form deposits of an attachment bond between the support structure and the sample. In this manner, by allowing the milled-away material to redeposit, one or more attachment bonds can be created between the sample and the non-milled portions of the support structure that hold the sample in place. Not only are these attachment bonds easy for the user to create / easily automatable because they are created without introducing precursor gases or liquids, but this process 200 can also be used to attach samples composed of highly reactive materials to the support structure.

[0045] At 212, the sample is optionally processed to prepare it for imaging and / or study. For example, a charged particle beam can be used to mill away portions of the sample to expose regions of interest in the sample, the sample can be polished to remove damage from the surface of the sample, or a combination thereof. In some embodiments, after imaging / studying the exposed surface, the sample can be subjected to one or more additional processes such that different regions of interest are exposed for imaging / studying. In some embodiments, when milling the sample at step 212, the charged particle beam is tilted such that the charged particle beam first mills through a portion of the support structure before it begins to remove portions of the sample. In this way, the portion of the support structure can serve as a protective cap to prevent draping of the exposed sample surface. Thus, in addition to creating an attachment bond without introducing a precursor gas, process 200 can also allow for the use of a protective cap without introducing a precursor gas. In some embodiments, processing the sample can include milling away the attachment bond between the sample and the sample manipulator such that the sample is disconnected from the sample manipulator. In other embodiments, processing the sample can include milling away a portion of the sample probe such that the tip of the sample probe remains attached to the sample and the remainder of the sample probe is disconnected from the sample.

[0046] At 214, the sample is imaged and / or studied. In various embodiments, imaging and / or studying the sample corresponds to performing one or more of the following: serial section tomography of regions of interest on the sample, enhanced charge coupled backscattered detector (CBS) analysis of regions of interest, and electron backscatter diffraction (EBSD) analysis of regions of interest. Steps 212 and 214 can be repeated such that multiple regions of interest within the sample can be imaged and / or studied.

[0047] Figure 3 and 7 is a visual flow chart illustrating an example process for performing sample extraction and protective cap placement for highly reactive materials in accordance with the present disclosure. Specifically, Figure 3 shows a series of captured images 300 that depict an example execution of the example process 200 described in the notes regarding Figure 2 the present disclosure.

[0048] Image 302 shows optionally creating a sample 320 from a sample body 322. Specifically, image 302 shows a state in which one or more volumes 324 of the sample body 322 surrounding the sample 320 are milled away using a charged particle beam (e.g., an ion beam). Image 304 shows a subsequent state of the example process in which a sample manipulator 326 is attached to the sample 320. For example, a deposition gas can be used or by Figure 5The associated attachment process attaches the sample 320 to the sample manipulator 326. Once the sample 320 is attached to the sample manipulator 326, the final portion 328 of the sample that previously connected the sample to the sample body is milled away. Once the sample 320 is completely detached from the sample body in this manner, the sample manipulator 326 can translate the sample 320 away from the sample body 322.

[0049] Image 306 shows a state in which a nested void 330 is prepared in the support structure 332. For example, a charged particle beam can be used to mill away material from the support structure 332. The nested void 330 can correspond to a hole, recess, cavity, or insertion volume into which a portion of the sample can be inserted. Although not shown in Image 306, in some embodiments, the nested void can correspond to a region adjacent to and / or abutting a raised structure / portion of the support structure such that when the sample is translated into the nested void, a portion of the sample is close to and / or abuts the raised structure / portion of the support structure. In various embodiments, the support structure 332 can correspond to one or more of a sample grid, a sample holder, or other structures that allow the sample to be imaged / studied when the sample is attached thereto. The support structure can be at least partially composed of many different materials, including but not limited to silicon, aluminum, copper, etc.

[0050] Image 308 shows a state in which at least a portion of the sample is positioned within the nested void 330 after the sample 320 has been translated, tilted, rotated, or otherwise manipulated relative to the support structure. The sample is shown attached to a movable sample manipulator 326 (i.e., a sample probe) that has been translated, tilted, and / or rotated such that at least a portion of the sample 320 is received within the nested void 330.

[0051] Image 310 shows the state of Image 308 in which a plurality of milling positions 334 have been mapped onto the image. Specifically, Image 310 shows a plurality of milling positions 334, each corresponding to a portion of the support structure 332 that will be milled using a charged particle beam. Image 312 shows the state of the process after a portion 334 of the sample holder 332 has been milled away and allows the milled material to redeposit to form an attachment bond 336 between the sample 320 and the support structure 332.

[0052] Figures 4A to 4C is a captured image that shows example results for sample extraction and protective cap placement for highly reactive materials according to the present disclosure and according to the prior art. Figure 4A is at Figure 3The sample 320 has been further processed to prepare it for imaging and / or study of an image 410 of the sample thereafter. By way of example, portions of the sample 320 have been milled away using a charged particle beam to expose a clean surface 412 of the region of interest in the sample, and then polished to remove damage from the surface of the sample. Specifically, Figure 4A Shows an example in which the portion of the sample 320 is removed and cleaned such that a clean reactive surface 412(a) (i.e., the clean surface of a portion of the sample composed of a reactive material) and a clean stable surface 412(b) (i.e., the clean surface of a portion of the sample composed of a non-reactive material) are exposed. In such embodiments where the sample is composed of both a stable material and a reactive material, milling may first be performed through the stable material such that the stable material acts as a cap that reduces the drape of the clean reactive surface 412(a). Alternatively, in some embodiments, milling may be performed such that portions of the support structure 322 are first milled through such that the support structure 322 acts as a cap that reduces the drape of the clean reactive surface 412(a). Using the processes described herein, high-quality EBSD maps and / or band contrast maps can be obtained for the clean surface 412 of highly reactive materials, which was not possible previously in the prior art.

[0053] Additionally, in some embodiments, the processes described herein have been shown to preserve the crystallinity of highly reactive materials, as evidenced by the acquired Kikuchi patterns of portions of such clean surfaces 408. Figure 4B Shows an image 420 in which a sample 422 has been inserted into a nested void 424 in a support structure 426 and attached using techniques according to the present disclosure. Figure 4B Further shown is a use 428 for assisting a user in processing and / or automatically processing and studying the region of interest in the sample 422.

[0054] Figure 4C Shows the results of sample extraction and protective cap placement for a highly reactive material using the prior art. As can be seen, when an attachment 432 is formed between the highly reactive sample 434 and the support structure 436, the sample 434 undergoes significant damage. This damage occurs at two separate steps in the prior art system. First, the sample 434 can be damaged by reacting with external materials (such as deposition gases, bonding liquids) introduced to form the attachment. Second, even if this introduction of the external material is not catastrophically damaging, the reaction between the external material and the highly reactive material 434 can cause the surface of the sample 434 to have subsequent catastrophic reactions when irradiated with a charged particle beam. As shown in the image 430, because of these reactions, the prior art for in-situ attachment of samples is not suitable for highly reactive materials.

[0055] Figure 5FIG. 500 is a flow chart of an illustrative process 500 for creating an attachment between a sample manipulator and a sample within a charged particle system. Process 500 may be implemented in example processes 200 - 400, example charged particle microscope setup 100, and / or implemented by computing architecture 150 described above, or implemented in other environments and architectures.

[0056] At 502, a high sputtering yield material is optionally attached to the sample manipulator. Specifically, a high sputtering yield material, such as copper, may be attached to the sample manipulator within the chamber of the charged particle system, outside of this chamber, or a combination thereof. For example, the high sputtering yield material may be attached to the probe portion of the sample manipulator using gas deposition attachment, where a precursor gas is introduced into the region between the sample manipulator and the high sputtering yield material, and then a charged particle beam is used to induce the deposition of the precursor gas to form an attachment bond. In another example process, the sample manipulator may be moved adjacent to the high sputtering yield material, the charged particle beam may be used to mill away portions of the high sputtering yield material near the sample, and the milled material may be allowed to precipitate to form one or more attachment bonds between the sample manipulator and the high sputtering yield material.

[0057] Alternatively, in some embodiments of the inventive process, instead of requiring step 502 to be performed, the sample manipulator includes a probe made of a high sputtering yield material (e.g., coated as such when purchased, or not coated and added in - situ or ex - situ when purchased).

[0058] At 504, the sample is brought close to the sample manipulator. Specifically, the sample and / or the sample manipulator may be moved such that a portion of the sample manipulator that will be attached to the sample (e.g., a probe, an intermediate body made of a high sputtering yield material attached in step 502, etc.) is within 10 microns of each other, within 1 micron of each other, or closer. For example, the sample and / or the sample manipulator may be attached to a moving assembly and / or otherwise configured to translate, tilt, and / or rotate.

[0059] At 506, a charged particle beam is applied to irradiate the high sputtering yield material. Specifically, the charged particle beam is used to mill away one or more portions of the high sputtering yield material, while leaving one or more other portions of the high sputtering yield material near the sample manipulator that remain un - milled. In this way, although some portions of the high sputtering yield material close to the sample are removed, there are still portions of the material within 10 microns of the sample, within 1 micron of the sample, or closer to the sample. For example, three portions located on the edge / surface of the high sputtering yield material may be milled, while two portions of the material between the three portions may remain un - milled.

[0060] At 508, redeposition of the milled high sputtering yield material is allowed to form an attachment bond between the sample and the sample manipulator. Although portions of the high sputtering yield material are milled away at step 506 and immediately thereafter, the sample is held in a constant position such that the material milled away is allowed to settle on the high sputtering yield material and / or the non-milled portions of the sample. In this way, the milled material is allowed to form interconnections to create a deposit of an attachment bond between the high sputtering yield material and the sample. By allowing the milled material to redeposit, one or more attachment bonds can be created between the sample and the non-milled portions of the high sputtering yield material that hold the sample in place. Not only are these attachment bonds easy for the user to create / easy to automate because they are created without introducing precursor gases or liquids, but this process 500 can also be used to attach samples made of highly reactive materials to a support structure. Additionally, this process 500 allows attachment bonds to be performed at low temperatures and / or in a vacuum without the need to develop a dedicated microscope mechanism or include a charged particle system and without the user having to learn a complex process.

[0061] At 510, the sample is optionally translated by the sample manipulator. For example, the sample manipulator can translate, tilt, and / or rotate the sample such that the sample is in a desired position within the charged particle system.

[0062] Figures 6A to 6C Different example embodiments for creating an attachment between a sample manipulator and a sample within a charged particle system are shown. For example, Figure 6A An example 610 is depicted where a sample 612 is attached to a sample manipulator 614, which corresponds to a sample probe made of a high sputtering yield material. In this way, when a portion 616 of the sample probe near the sample 612 is milled away, the milled material is at least partially redeposited to form an attachment structure 618 between the sample 612 and the sample manipulator 614.

[0063] Figure 6B An example 640 is depicted where a sample 642 is attached to a sample manipulator corresponding to a sample probe 644 coated with a high sputtering yield material 646. In this way, when a portion 648 of the coating near the sample 642 is milled away, the milled material is at least partially redeposited to form an attachment structure 650 between the sample 642 and the sample manipulator. Figure 6C An example 660 is depicted where a sample 662 is attached to a sample manipulator corresponding to a sample probe 664 made of a high sputtering yield material attached to an intermediate body 666. When a portion 668 of the intermediate body 666 near the sample 642 is milled away, at least some of the milled material is redeposited to form an attachment structure 670 between the sample 662 and the intermediate body 666.

[0064] Figure 7 Displays a series of images 700 that illustrate an example execution of an example process for sample extraction and placement of a protective cap for highly reactive materials using a sample holder with beveled edges. Image 702 shows an example sample holder 720 with beveled edges 722. According to the present invention, the beveled edge can be any angle less than 90 degrees. In some embodiments, a charged particle beam can be used to mill away portions of the sample holder 720 to create the beveled edge 722. Image 704 shows a state in which a nested void 724 is prepared in the support structure 720 near the beveled edge 722. For example, a charged particle beam can be used to mill away material from the support structure 720 such that a hole, recess, or insertion volume is created in which a portion of the sample can be inserted.

[0065] Image 706 shows the sample 726 being translated using a sample manipulator 728 during the process such that at least a portion of the sample 726 is positioned within the nested void 724. Specifically, image 706 shows an embodiment in which the sample 726 has been attached to the sample manipulator 728 using an intermediate body 730 made of a high sputter yield material, as shown and described in connection with Figure 5 and 6C associated therewith. Image 708 shows the state after the sample 726 has been translated such that at least a portion is positioned within the nested void 724 and then the sample 726 is attached to the sample holder 720 by milling away the portion of the sample holder 732 near the sample such that the milled material is redeposited, thereby forming an attachment structure between the sample 726 and the sample holder 720.

[0066] Image 710 shows a cross-section of the state depicted in image 708. Image 710 shows a cross-section of the sample 726 and a thin portion of the sample holder 734 that extends along the surface of the sample 726. Image 712 shows a state in which a charged particle beam 736 is used to mill away portions of the sample 726 and the thin portion of the sample holder 734 along a plane 738 to expose the surface of interest 740. In this way, the thin portion of the sample holder 734 acts as a protective cap onto which the charged particle beam 736 first impinges, thus reducing the curtaining effect on the area of interest 740. In some embodiments, an electron beam 742 can then optionally be used to image or otherwise study the area of interest 740.

[0067] Examples of the inventive subject matter according to the present disclosure are described in the paragraphs listed below.

[0068] A1. A method for performing sample extraction and protective cap placement for highly reactive materials within a charged particle microscope system, the method comprising: preparing a nested void translation in a support structure; translating at least a portion of a sample into the nested void; and milling material from a region of the support structure that defines the nested void such that at least some of the material milled from the support structure is redeposited to form an attachment bond between the sample and the remaining portion of the support structure.

[0069] A2. The method according to paragraph A1, wherein preparing the nested void comprises milling away a volume of the support structure, the volume being capable of receiving at least a portion of the sample.

[0070] A2.1. The method according to paragraph A2, wherein the nested void is a hole, and wherein translating the at least a portion of the sample into the nested void corresponds to translating the sample such that at least a portion of the sample is inside the hole.

[0071] A2.2. The method according to any one of paragraphs A2 to A2.1, wherein the nested void is configured such that when the attachment bond is formed between the sample and the support structure, at least a portion of the sample is positioned at a location where the milled - away volume of the sample was located.

[0072] A2.3. The method according to any one of paragraphs A2 to A2.2, wherein the volume of the support structure is milled away using a focused ion beam.

[0073] A3. The method according to any one of paragraphs A1 to A2.3, wherein the method further comprises performing one or more of the following: serial section tomography of the sample; enhanced insertable backscattered detector (CBS) analysis of the sample; chemical analysis, SIMS analysis, electron beam (EDX) analysis, Raman analysis, and electron backscatter diffraction (EBSD) analysis of the sample.

[0074] A3.1. The method according to paragraph A3, wherein the method comprises milling away a portion of the sample to expose a surface of interest and imaging at least a portion of the surface of interest.

[0075] A3.1.1. The method according to paragraph A3.1, wherein the milling is performed using a focused ion beam.

[0076] A3.1.2. The method according to any one of paragraphs A3.1 to A3.1.1, wherein at least a portion of the support structure serves as a protective cap during the milling of the sample.

[0077] A3.1.2.1. The method according to paragraph A3.1.2, wherein using the portion of the support structure as a protective cap includes milling and positioning the focused ion beam such that the portion of the support structure is milled away before the portion of the sample is milled away by the focused ion beam.

[0078] A3.1.2.1.1. The method according to paragraph A3.1.2.1, wherein the portion of the sample is milled away using a high-current milling machine with FIB or plasma FIB.

[0079] A3.1.2.2. The method according to any one of paragraphs A3.1.2 to A3.1.2.1.1, wherein using the portion of the support structure as a protective cap prevents the tail of the focused ion beam from milling away a portion of the sample.

[0080] A3.1.3. The method according to any one of paragraphs A3.1 to A3.1.2.2, wherein the imaging includes irradiating at least a portion of the surface of interest with an electron beam.

[0081] A3.1.4. The method according to any one of paragraphs A3.1 to A3.1.3, wherein the process further includes milling away an additional portion of the sample to expose an additional surface of interest.

[0082] A3.1.5. The method according to any one of paragraphs A3.1 to A3.1.4, wherein the process further includes milling away a plurality of additional portions of the sample to expose a plurality of additional surfaces of interest.

[0083] A3.1.6. The method according to any one of paragraphs A3.1 to A3.1.5, wherein milling away the portion of the sample is performed at least partially using a rocking milling machine.

[0084] A4. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is a sample grid.

[0085] A4.1. The method according to paragraph A4, wherein the sample grid is a TEM sample grid.

[0086] A5. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is a sample holder.

[0087] A6. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is at least partially composed of silicon.

[0088] A7. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is an aluminum block.

[0089] A8. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is made of an inert material that is not reactive to the (said) focused ion beam.

[0090] A9. The method according to any one of paragraphs A1 to A3.1.6, wherein the support structure is an inclined holder having an inclined edge.

[0091] A9.1. The method according to paragraph A9, wherein at least a part of the inclined holder extends beyond the sample when the sample is inserted into the nested void.

[0092] A9.2. The method according to any one of paragraphs A9 to A9.1, further comprising milling away a section of the sample, including milling through the inclined edge using the inclined edge as a protective cap.

[0093] A9.3. The method according to any one of paragraphs A9 to A9.2, wherein the inclined edge is milled at a 45-degree angle.

[0094] A9.4. The method according to any one of paragraphs A9 to A9.3, wherein you can create the inclined edge, or it can be a commercially available part.

[0095] A10. The method according to any one of paragraphs A1 to A9.4, wherein the sample is attached to the sample probe by an attachment bond, and wherein translating at least the portion of the sample into the nested void includes translating the sample probe such that at least the portion of the sample is translated into the nested void.

[0096] A10.1. The method according to paragraph A10, further comprising milling away the attachment bond such that the sample is disconnected from the sample probe.

[0097] A10.2. The method according to paragraph A10, further comprising milling away a part of the sample probe such that the tip of the sample probe remains attached to the sample and the rest of the sample probe is disconnected from the sample.

[0098] A11. The method according to any one of paragraphs A1 to A10.2, further comprising the step of preparing the sample from the specimen.

[0099] A11.1. The method according to paragraph A11, wherein preparing the sample from the specimen comprises the steps of: milling away a portion of the specimen surrounding the area of interest; attaching a sample probe to the area of interest; and milling away a portion of the specimen such that the area of interest is no longer attached to the specimen.

[0100] A11.1.1. The method according to paragraph A11.1, wherein preparing the sample from the specimen further comprises translating the sample probe such that the area of interest is moved away from the specimen.

[0101] A11.1.2. The method according to any one of paragraphs A11.1 to A11.1.1, wherein the area of interest corresponds to the sample.

[0102] A11.1.3. The method according to any one of paragraphs A11.1 to A11.1.2, wherein attaching the sample probe to the area of interest comprises the method according to any one of paragraphs B1 to B14.2.2.2.2.1.

[0103] A12. The method according to any one of paragraphs A1 to A11.1.3, wherein the specimen corresponds to a battery or a part of a battery.

[0104] A12.1. The method according to paragraph A12, wherein the specimen corresponds to a lithium battery, a lithium-ion battery, a battery anode, a battery cathode, a battery separator, or a combination thereof.

[0105] A13. The method according to any one of paragraphs A1 to A12.1, wherein the material comprises at least one of lithium, magnesium, lithium polymer, lithium manganese oxide, lithium cobalt oxide, and lithium sulfide.

[0106] A14. The method according to any one of paragraphs A1 to A13, wherein one of a focused ion beam and an electron beam is used to perform the milling.

[0107] A14.1. The method according to paragraph A14, wherein the ion beam is a plasma focused ion beam.

[0108] B1. A method for creating an attachment between a sample manipulator and a sample within a charged particle system, the method comprising: translating the sample manipulator such that it approaches the sample, wherein a portion of the sample manipulator approaching the sample is made of a high sputtering yield material; and milling the high sputtering yield material using a charged particle beam such that a portion of the high sputtering yield material is removed from the sample manipulator, and wherein at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample.

[0109] B1.1. According to the method described in paragraph B1, wherein when irradiating with specific ionic substances and voltages other than silicon or tungsten, the high sputtering yield material corresponds to a material that produces a larger number of atoms per ion.

[0110] B1.1.1. According to the method described in paragraph B1.1, wherein when irradiating the material with a 30 kV focused ion beam, the high sputtering yield material corresponds to an emission rate of greater than 5, 7, 8, or 10 atoms per ion.

[0111] B1.1.1.1. According to the method described in paragraph B1.1.1, wherein the 30 kV focused ion beam is one of Ga+, Xe+, Ar, N+, Cs+, Bi+, or O+ focused ion beams.

[0112] B1.2. According to the method described in any one of paragraphs B1 to B1.1.1.1, wherein the high sputtering yield material is copper or brass.

[0113] B2. According to the method described in any one of paragraphs B1 to B1.2, wherein the translation of the sample manipulator includes translating the sample manipulator such that the portion made of the high sputtering yield material is within 10 micrometers.

[0114] B2.1. According to the method described in paragraph B2, wherein the translation of the sample manipulator includes translating the sample manipulator such that the portion made of the high sputtering yield material is within one micrometer.

[0115] B3. According to the method described in any one of paragraphs B1 to B2.1, wherein the sample manipulator includes a probe made of the high sputtering yield material.

[0116] B4. According to the method described in any one of paragraphs B1 to B2.1, wherein the sample manipulator includes a probe coated with the high sputtering yield material.

[0117] B4.1. According to the method described in paragraph B4, wherein irradiating the high sputtering yield material includes milling away the portion of the coating close to the sample.

[0118] B5. According to the method described in any one of paragraphs B1 to B2.1, wherein the sample manipulator includes an intermediate body attached to the probe, and wherein the intermediate body is made of the high sputtering yield material.

[0119] B5.1. According to the method described in paragraph B5, wherein the intermediate body is attached to the probe portion of the sample manipulator.

[0120] B5.1.1. The method according to paragraph B5.1, wherein the intermediate body is attached to the probe portion of the sample manipulator by gas deposition.

[0121] B5.1.2. The method according to paragraph B5.1, wherein the intermediate body is attached to the probe portion of the sample manipulator by a process comprising:

[0122] Translating the probe portion so that it is close to the intermediate body; and

[0123] Milling a portion of the intermediate body close to the probe with the charged particle beam, and at least some of the intermediate body removed is redeposited to form an attachment between the probe portion and the intermediate body.

[0124] B6. The method according to any one of paragraphs B1 to B5.1.2, wherein the charged particle beam is a focused ion beam.

[0125] B6.1. The method according to paragraph B6, wherein the charged particle beam is a plasma focused ion beam.

[0126] B7. The method according to any one of paragraphs B1 to B5.1.2, wherein the charged particle beam is an electron beam.

[0127] B8. The method according to any one of paragraphs B1 to B7, wherein the method for creating an attachment between the sample manipulator and the sample within the charged particle system requires a reduced amount of precursor gas compared to traditional attachment methods.

[0128] B9. The method according to any one of paragraphs B1 to B8, wherein the attachment between the sample manipulator and the sample is formed without adding additional precursor gas to the system.

[0129] B10. The method according to any one of paragraphs B8 or B9, wherein the precursor gas comprises platinum.

[0130] B11. The method according to any one of paragraphs B1 to B10, wherein the method is performed in the charged particle system at a low temperature.

[0131] B12. The method according to any one of paragraphs B1 to B11, wherein the method is performed in the charged particle system under vacuum.

[0132] B13. The method according to any one of paragraphs B1 to B12, wherein the sample is a wafer.

[0133] B14. The method according to any one of paragraphs B1 to B13, wherein milling the high sputtering yield material includes milling a plurality of positions on the high sputtering yield material close to the sample.

[0134] B14.1. The method according to paragraph B14, wherein each of the plurality of positions is located at an edge of the high sputtering yield material close to the sample.

[0135] B14.2. The method according to any one of paragraphs B14 to B14.1, wherein at least one non-milled area of the high sputtering yield material along the edge close to the sample is between the plurality of positions.

[0136] B14.2.1. The method according to paragraph B14.2, wherein at least some of the removed high sputtering yield material are redeposited to form the attachment between the sample and the at least one non-milled area of the high sputtering yield material along the edge close to the sample.

[0137] B14.2.2. The method according to any one of paragraphs B14.2 to B14.2.1, wherein there are a plurality of non-milled areas of the high sputtering yield material along the edge of the sample close to the sample.

[0138] B14.2.2.1. The method according to paragraph B14.2.2, wherein at least some of the removed high sputtering yield material are redeposited to form the attachment between the sample and the at least one non-milled area of the high sputtering yield material along the edge close to the sample among the plurality of non-milled areas.

[0139] B14.2.2.2. The method according to any one of paragraphs B14.2.2 to B14.2.2.1, wherein at least some of the removed high sputtering yield material are redeposited to form a plurality of attachments between the sample and the high sputtering yield material.

[0140] B14.2.2.2.1. The method according to paragraph B14.2.2.2, wherein each of the plurality of attachments connects the sample to a corresponding one of the at least one non-milled area of the high sputtering yield material along the edge close to the sample.

[0141] B14.2.2.2.2. The method according to any one of paragraphs B14.2.2.2 to B14.2.2.2.1, wherein the at least one non-milled area of the high sputtering yield material along the edge close to the sample among the plurality of non-milled areas.

[0142] B14.2.2.2.2.1. According to the method described in paragraph B14.2.2.2.2, at least four attachments are formed between the sample and the corresponding area of the high sputtering yield material that is not milled away along the edge close to the sample.

[0143] C1. A charged particle system, the system comprising: a charged particle emitter configured to emit charged particles towards a sample; a sample holder configured to support the sample; an optical column configured to direct the charged particles to be incident on the sample; a detector system configured to detect emissions from the sample caused by irradiation of the charged particles; one or more processors; and a memory storing non - transitory computer - readable instructions, the non - transitory computer - readable instructions when executed by the one or more processors cause the one or more processors to perform the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

[0144] C2. The charged particle system according to paragraph C1, further comprising a vacuum chamber for accommodating the sample.

[0145] C2.1. The charged particle system according to paragraph C2, wherein the instructions cause the one or more processors to perform the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1 when the sample is in a vacuum.

[0146] C2.2. The charged particle system according to paragraph C2, wherein the instructions cause the one or more processors to perform the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1 without breaking the vacuum in the vacuum chamber.

[0147] C3. The charged particle system according to any one of paragraphs C1 to C2.2, wherein the instructions cause the one or more processors to perform the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1 when the sample is at a low temperature.

[0148] D1. Use of a system according to any one of paragraphs C1 to C3, the system for performing the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

[0149] E1. A non - transitory computer - readable medium storing instructions which, when executed by a processor, cause the processor to initiate performance of the method according to any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

[0150] F1. Use of a non - transitory computer - readable medium as described in paragraph E1, the non - transitory computer - readable medium being configured to perform a method as described in any one of paragraphs A1 to A12.7 and / or B1 to B14.2.2.2.2.1.

Claims

1. A method for creating an attachment between a sample manipulator and a sample within a charged particle system, the method comprising: Translate the sample manipulator so that it approaches the sample, wherein the portion of the sample manipulator approaching the sample is made of a high sputtering yield material; and Mill the high sputtering yield material using a charged particle beam so that a portion of the high sputtering yield material is removed from the sample manipulator, and wherein at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample, wherein the sample manipulator includes an intermediate body attached to a probe, wherein the intermediate body is made of the high sputtering yield material, and wherein the intermediate body is attached to the probe portion of the sample manipulator by a process including: Translate the probe portion so that it approaches the intermediate body; and Mill the portion of the intermediate body approaching the probe using the charged particle beam, wherein at least some of the removed intermediate body is redeposited to form an attachment between the probe portion and the intermediate body, and When irradiating the high sputtering yield material with a 30 kV focused ion beam, the high sputtering yield material corresponds to an emission rate of greater than 5 atoms per ion.

2. The method according to claim 1, wherein the high sputtering yield material is copper.

3. The method according to claim 1, wherein translating the sample manipulator includes translating the sample manipulator so that the portion made of the high sputtering yield material approaches the sample within 10 micrometers.

4. The method according to claim 3, wherein translating the sample manipulator includes translating the sample manipulator so that the portion made of the high sputtering yield material approaches the sample within 1 micrometer.

5. The method according to claim 1, wherein the sample manipulator includes a probe made of the high sputtering yield material.

6. The method according to claim 1, wherein the sample manipulator includes a probe coated with the high sputtering yield material, and wherein irradiating the high sputtering yield material includes milling off the portion of the coating approaching the sample.

7. The method according to claim 1, wherein the intermediate body is attached to the probe portion of the sample manipulator by gas deposition.

8. The method according to claim 1, wherein the method is performed in the charged particle system at a low temperature.

9. The method according to claim 1, wherein milling the high sputtering yield material includes milling a plurality of positions on the high sputtering yield material approaching the sample, and wherein each of the plurality of positions is located at the edge of the high sputtering yield material approaching the sample.

10. The method according to claim 9, wherein at least one non-milled zone of the high sputtering yield material along the edge approaching the sample is between the plurality of positions, and wherein at least some of the removed high sputtering yield material is redeposited to form at least one attachment between the sample and the at least one non-milled zone of the high sputtering yield material along the edge approaching the sample.

11. The method according to claim 9, wherein there are a plurality of regions of the high sputtering yield material that are not milled away along the edge close to the sample, and wherein at least some of the removed high sputtering yield material is redeposited to form a plurality of attachments between the sample and individual regions of the at least one region of the high sputtering yield material that is not milled away along the edge close to the sample.

12. A non - transitory computer - readable medium storing instructions that, when executed by a processor, cause the processor to initiate execution of the following steps: Translate a sample manipulator so that it approaches the sample, wherein a portion of the sample manipulator close to the sample is made of a high sputtering yield material; and Mill the high sputtering yield material with a charged particle beam so that a portion of the high sputtering yield material is removed from the sample manipulator, and wherein at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample, wherein the sample manipulator includes an intermediate body attached to a probe, and wherein the intermediate body is made of the high sputtering yield material, wherein the intermediate body is attached to the probe portion of the sample manipulator by gas deposition, and when irradiating the high sputtering yield material with a 30 kV focused ion beam, the high sputtering yield material has an emission rate of greater than 5 atoms per ion.

13. A method for creating an attachment between a sample manipulator and a sample within a charged particle system, the method comprising: Translate a sample manipulator so that it approaches the sample, wherein a portion of the sample manipulator close to the sample is made of a high sputtering yield material; and Mill the high sputtering yield material with a charged particle beam so that a portion of the high sputtering yield material is removed from the sample manipulator, and wherein at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample, wherein milling the high sputtering yield material includes milling a plurality of positions on the high sputtering yield material close to the sample, wherein each of the plurality of positions is located at the edge of the high sputtering yield material close to the sample, wherein at least one region of the high sputtering yield material that is not milled away along the edge close to the sample is between the plurality of positions, and wherein at least some of the removed high sputtering yield material is redeposited to form at least one attachment between the sample and the at least one region of the high sputtering yield material that is not milled away along the edge close to the sample, and when irradiating the high sputtering yield material with a 30 kV focused ion beam, the high sputtering yield material has an emission rate of greater than 5 atoms per ion.

14. A method for creating an attachment between a sample manipulator and a sample within a charged particle system, the method comprising: Translate a sample manipulator so that it approaches the sample, wherein a portion of the sample manipulator close to the sample is made of a high sputtering yield material; and Milling the high sputtering yield material with a charged particle beam such that a portion of the high sputtering yield material is removed from the sample manipulator, and wherein at least some of the removed high sputtering yield material is redeposited to form an attachment between the sample manipulator and the sample, wherein milling the high sputtering yield material includes milling a plurality of locations on the high sputtering yield material near the sample, wherein each of the plurality of locations is located at an edge of the high sputtering yield material near the sample, wherein there are a plurality of regions of the high sputtering yield material that are not milled away along the edge near the sample, and wherein at least some of the removed high sputtering yield material is redeposited to form a plurality of attachments between the sample and individual regions of the at least one of the regions of the high sputtering yield material that are not milled away along the edge near the sample, and when the high sputtering yield material is irradiated with a 30 kV focused ion beam, the high sputtering yield material corresponds to an emission rate of greater than 5 atoms per ion.

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