Systems and methods for performing sample extraction of highly reactive materials

Abstract

Disclosed herein are methods and systems for performing sample extraction and protective cap placement for highly reactive materials within a charged particle microscope system. The methods include preparing a nested void in a support structure; transferring 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. Milling the material from the region of the support structure causes at least some of the removed material to redeposit to form an adhesive bond between the sample and a remaining portion of the support structure. In various embodiments, the sample can then be investigated using one or more of serial section tomography of the sample, enhanced insertable backscatter detector (CBS) analysis of the sample, and electron backscatter diffraction (EBSD) analysis of the sample.

Description

BACKGROUND

[0001] In scanning and transmission charged particle microscopy, a charged particle beam is used to image or otherwise study a region of interest on a sample. In many cases, prior to the region of interest can be imaged and / or studied, it is often necessary to prepare and / or manipulate the sample within the system to allow the region of interest to be exposed or otherwise prepared. In current systems, this preparation often involves one or more of the following: using a charged particle beam to prepare a sample from a larger specimen, attaching the sample to a manipulation probe to allow the sample to be transferred within the microscope system, and attaching the sample to a sample holder so that the region of interest on the sample can be processed, imaged and / or otherwise studied.

[0002] In current systems, a precursor gas or a deposition liquid is used to attach the sample to the probe and / or sample holder. Specifically, in some attachment methods, a precursor gas is introduced into a volume surrounding the sample, where the gas molecules form a deposit on the sample, probe and / or sample holder when illuminated by a charged particle beam. In another existing attachment method, a liquid is first introduced to the sample, probe and / or sample holder, and the liquid is illuminated with a charged particle beam so that it solidifies, forming an attachment bond between the sample and the probe and / or sample holder. However, while these systems are suitable for many general applications, they are each subject to drawbacks that make them unsuitable for certain microscopy studies.

[0003] For example, charged particle microscope systems study samples in a sealed chamber to reduce contamination of optical components, reduce the effect of unwanted particles on the charged particle beam, and to have 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 specially tailored mechanisms that complicate the design and implementation of new charged particle systems, while also adding complex processing steps that are difficult for new users to implement accurately. Finally, for highly reactive samples, traditional precursor gases cannot be used because the introduction of the gas can cause the sample surface to deteriorate and / or cause the sample to be more reactive to the charged particle beam when subsequently polished or imaged after attachment. Therefore, it is desirable to have new attachment and sample manipulation systems and processes to allow for imaging and studying of highly reactive materials. SUMMARY

[0004] Disclosed herein are methods and systems for performing sample extraction and protective cap placement on highly reactive materials within a charged particle microscope system. The methods include preparing a nested void in a support structure; transferring 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. Milling the material from the region of the support structure causes at least some of the removed material to redeposit to form an adhesive bond between the sample and a remaining portion of the support structure. In various embodiments, the sample can then be investigated using one or more of serial section tomography of the sample, enhanced insertable backscatter detector (CBS) analysis of the sample, and electron backscatter diffraction (EBSD) analysis of the sample.

[0005] A system for performing sample extraction and protective cap placement on highly reactive materials within a charged particle system according to the present disclosure can include a charged particle emitter configured to emit charged particles toward a sample; a sample holder configured to support a sample; an optical column configured to direct charged particles incident on a sample; and a detector system configured to detect emissions from a sample due to illumination by charged particles. The system also 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 prepare a nested void in a support structure, transfer at least a portion of a sample into the nested void; and mill material from a region of the support structure that defines the nested void. BRIEF DESCRIPTION OF DRAWINGS

[0006] The detailed description is described with reference to the accompanying figures. In the figures, the left-most digit(s) of each reference number identifies the figure in which that reference number first appears. The use of the same reference numbers in different figures indicates similar or identical items.

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

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

[0009] Figure 3 A series of captured images demonstrating example performance of sample extraction and protective cap placement on highly reactive materials within a charged particle microscope system.

[0010] Figures 4A to 4Ccaptured images showing example results of sample extraction and protective cover placement on a highly reactive material according to the present disclosure.

[0011] Figure 5 A flowchart showing a schematic 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 showing creating an attachment between a sample manipulator and a sample in a charged particle system.

[0013] Figure 7 A series of images showing example performance of an example process for sample extraction and protective cover placement on a highly reactive material using a sample holder with a beveled edge.

[0014] Throughout the drawings, like reference numerals will be used to refer to like or corresponding parts throughout the several views. DETAILED DESCRIPTION

[0015] Methods and systems for performing sample extraction and protective cover placement on 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, a sample is transferred such that at least a portion of the sample is within the nested void, and then material from a region of the support structure that defines the nested void is abraded away. The material from the region of the support structure is located in the vicinity of the sample such that at least some of the removed material redeposits to form one or more attachment bonds between the sample and the remaining portion of the support structure. In this way, the sample can be attached to the 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 through passive redeposition of the abraded material, there is much less opportunity for reaction and / or other types of damage to the sample. This allows samples composed of highly reactive materials, such as those found in lithium-based battery technology, to be attached to a sample holder without damaging the sample. Once the sample is attached to the sample holder in this way, 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 backscatter detector (CBS) analysis of the sample, and electron backscatter diffraction (EBSD) analysis of the sample.

[0016] Additionally, methods and systems for creating an attachment between a sample manipulator and a sample within a charged particle system are also disclosed herein. In particular, the present disclosure includes methods and systems in which a sample is attached to a holding or manipulator by irradiating a high sputtering rate material near the sample. Initially, a transfer sample manipulator is brought such that a portion of the manipulator made of a high sputtering rate material is located near the sample (e.g., within microns). Then, a charged particle beam is used to mill away the region of high sputtering rate material near the sample such that at least some of the removed high sputtering rate material is redeposited to form an attachment between the sample manipulator and the sample. According to the present invention, a high sputtering rate material corresponds to a material that produces a greater number of atoms per ion than silicon or tungsten when irradiated with a particular ion beam species and voltage. For example, a high sputtering rate material is a high sputtering rate material defined as a material that emits greater than 5, 7, 8, or 10 atoms per ion when the material is irradiated with a 30 kV Ga+ focused ion beam (such as copper or zinc).

[0017] Generally, in the drawings, elements that can 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 required for all examples of the present disclosure, and elements shown in solid lines can be omitted from a particular example without departing from the scope of the present disclosure.

[0018] Figure 1 An example system 100 for sample extraction and protective cap placement on high reactivity materials, and / or for creating an attachment between a sample manipulator and a sample within a charged particle microscope system is shown. In particular, 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 on high reactivity materials. Note that the present invention is not limited to environments that include a microscope, and in some embodiments, the environment 100 can include a different type of system configured to manipulate and / or otherwise examine the sample 108.

[0019] The example microscope system 104 can 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 low temperature 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 that includes a STEM column 110 and a FIB column 112.

[0020] Figure 1The example microscope system 104 is depicted as including a STEM column 110 for illuminating a sample 108 with a charged particle beam 114. The STEM column 110 includes an electron source 116 (e.g., a hot electron source, a Schottky emission source, a field emission source, etc.) that 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 travels from the electron source 116 along a length of the example microscope system 104 and through the sample 108. While Figure 1 The example microscope system 104 is depicted as including an electron source 116, but in other embodiments, the STEM column 110 can include a charged particle source configured to emit a plurality of charged particles toward the sample 108, such as an ion source.

[0021] An accelerator lens 120 accelerates / decelerates, focuses, and / or directs the electron beam 114 toward an electron focusing column 122. The electron focusing column 122 focuses the electron beam 114 such that it is incident on at least a portion of the sample 108. Additionally, the focusing column 122 can correct and / or tune aberrations (e.g., geometric aberrations, chromatic aberrations) of the electron beam 114. In some embodiments, the electron focusing column 122 can include one or more of apertures, deflectors, transfer lenses, scanning coils, condenser lenses, objective lenses, etc. that together focus the electrons from the electron source 116 into a small spot on the sample 108. By adjusting the electron beam direction with the deflectors and / or scanning coils, different locations of the sample 108 can be scanned. In this manner, the electron beam 114 can act as an imaging beam that is scanned across a surface layer of the sample (i.e., a surface of a layer proximate the STEM column 104 and / or a surface of a layer that is illuminated by the electron beam 114). This illumination of the surface layer of the sample 108 causes constituent electrons of the electron beam 114 to interact with constituent elements / molecules / features of the sample such that the constituent elements / molecules / features cause emissions 124 to be emitted from the sample 108. The particular emissions that are released are based on the corresponding elements / molecules / features that caused them to be emitted, such that the emissions can be analyzed to determine information about the corresponding elements / molecules / features. Additionally, while Figure 1 The emissions 124 are shown as traveling downstream of the sample 108, but one of skill in the art will appreciate that the emissions can be released in other directions, including but not limited to toward the charged particle source 116.

[0022] Figure 1Also shown are detector systems 126(a) and 126(b) for detecting emissions 124 produced by the electron beam 114 incident on the sample 108. The detector systems 126 can include one or more detectors positioned or otherwise configured to detect such emissions. For example, a charged particle system according to the present disclosure can contain a detector system 126(a) positioned below the sample 108, a detector system 126(b) positioned above the sample 108, or both. In various embodiments, different detectors and / or different portions of a single detector can be configured to detect different types of emissions, or configured such that the parameters of the emissions detected by the different detectors and / or different portions are different. The detector systems 126 are also 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] While Figure 1 The example microscope system 104 is also depicted as containing a FIB column 112 for removing portions of the sample 108 or other object in the microscope chamber 130. For example, the FIB column 112 can be used to mill away portions of a sample body to reveal or otherwise create the sample 108. In other embodiments, the example microscope system 104 can contain other types of layering components, such as lasers, mechanical blades (e.g., diamond blades), electron beams, etc. The FIB column 112 is shown as containing 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 that travels from the charged particle emitter 132 and through the sample 108. The FIB column 112 also contains an ion focusing column 138 that includes one or more of apertures, deflectors, relay lenses, scanning coils, condenser lenses, objective lenses, etc. that together focus the ions from the charged particle emitter 132 to a small spot on the sample 108. In this way, the elements in the ion focusing column 138 can cause the ions emitted by the charged particle emitter 132 to mill away or otherwise remove one or more portions of the sample 108 or other body. For example, during slice and view imaging, the FIB column 112 can be configured such that a surface layer of the sample 108 having a known thickness is removed from the sample 108 between image acquisitions.

[0025] Figure 1The example microscope system 104 is also shown as 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 can translate, rotate, and / or tilt the sample 108 relative to the example microscope system 104. For example, the sample holder 140 can include a grid or structure to which a sample or specimen will be attached and / or otherwise held. Additionally, the sample manipulator 108 is a mechanism in the microscope chamber 130 that is capable of interacting with the sample 108 such that the sample can be translated, angled, 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 can be sealed from the microscope chamber 130, and can allow the sample holder 140 to be retracted therein such that a user can access and / or interact with the sample holder 140 while it is in 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 in the middle are merely illustrative, and are not intended to limit the scope of the present disclosure. Computing systems and devices can include any combination of hardware or software that can perform the indicated functions, including computers, network devices, internet appliances, PDAs, wireless telephones, controllers, oscilloscopes, amplifiers, etc. The computing devices 128 can also be connected to other devices not shown, or can operate as a stand-alone system.

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

[0028] Additionally, the computing device 128 is configured to control the FIB column 112, the sample manipulator 106, and / or the sample holder 140 to allow sample extraction and protective cap placement to be performed on high reactivity materials within the charged particle microscope system 104. For example, the computing device 128 can use the plurality of ions 134 to cause the FIB column 112 to mill a nested void in a support structure (e.g., a sample grid, a sample holder, or other structure that allows a sample to be imaged / studied when attached thereto). One or more user selections, automated procedures, or a combination thereof can allow the computing device 128 to cause the sample holder 140 or the sample manipulation device 106 to be transferred (e.g., translated, angled, and / or rotated) such that at least a portion of the sample 108 is positioned within the nested void. Once the sample 108 is at least partially positioned within the nested void, the computing device 128 can cause the FIB column 112 to mill away portions of the sample and / or portions of the support structure that define the nest. The user selections, automated procedures, or a combination thereof select portions of the support structure to be milled in this manner such that the milled material redeposits to form an adhesive bond between the support structure and the portion of the sample 108 in the nested void. 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 material into the microscope chamber 130. In some embodiments, the computing device 128 can also be configured to cause the example microscope system 104 to prepare the sample 108 prior to attachment (e.g., remove the sample from a larger sample body, reveal a surface / structure of interest), process the sample to prepare it for imaging / study, or perform imaging / study on one or more regions of the sample 108.

[0029] Alternatively or additionally, the computing device 128 can be configured to create one or more attachments between the sample manipulator 106 and the sample 108 within the charged particle system 104 without the need to add additional deposition gas or other material into the microscope chamber 130. For example, the computing device 128 can cause a high sputter rate material (e.g., copper) to be positioned near the sample 108. The high sputter rate material can optionally be attached to the sample manipulator, which itself can include a high sputter rate material (e.g., purchased with such a coating, or purchased without the addition of a coating through in-situ or ex-situ deposition).

[0030] User selection, an automated program, or a combination thereof can cause the computing device 128 to activate the FIB column 112 to mill away portions of the high sputter rate material proximate to the sample, while leaving one or more other portions of the high sputter rate material located proximate to the sample manipulator to remain unmilled. In this way, as some portions of the high sputter rate material proximate to the sample are removed, there remains a residual portion of material that is still within 10 microns, 1 micron, or closer to the sample. Thus, when the milled high sputter rate material is redeposited, it forms one or more adhesive bonds between the sample and the sample manipulator.

[0031] Figure 1 Also included is a diagram that shows an example computing architecture 150 of the computing device 128. The example computing architecture 150 illustrates additional details of hardware and software components that can be utilized to implement the techniques described in this disclosure. Those skilled in the art will appreciate that the computing architecture 150 can be implemented in a single computing device 128 or can be distributed across multiple computing devices. For example, various modules and / or data structures depicted in the computing architecture 150 can be executed and / or stored on different computing devices 128. In this way, it is within the scope of the present disclosure for different process steps of the inventive methods disclosed herein to be run and / or performed by separate computing devices 128 in various orders. 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, functionality of some of the illustrated components can not be provided and / or additional functionality can be available.

[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. While not intended to be limiting, the example computing architecture 150 is shown to include a control module 156 stored in the memory 154. As used herein, the term “module” is intended to represent an example partitioning of executable instructions for purposes of discussion, and is not intended to represent any type of requirement or required method, manner, or organization. Thus, while various “modules” are described, their functionality and / or similar functionality can be arranged in different ways (e.g., combined into a fewer number of modules, broken into a larger number of modules, etc.). Additionally, while particular functionality and modules are described herein as being implemented by software and / or firmware executable on a processor, in other examples, any or all of the modules can be implemented in whole or in part by hardware (e.g., special purpose processing units, etc.) to perform the described functionality. As discussed above in various implementations, the modules associated with the example computing architecture 150 described herein can be executed across multiple computing devices 128.

[0033] The control module 156 can be executed by the processor(s) 152 to cause the computing device 128 and / or the example microscope system 104 to take one or more actions and / or perform a function or maintenance of the system. In some embodiments, the control module 156 can cause the example 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 example microscope system 204 to perform such a process using the example process described in the discussion of Figure 2 Alternatively or additionally, the control module 156 can be configured to cause the example 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 requiring additional deposition gas or other material to be added to the microscope chamber 130. For example, the control module 156 can cause the example microscope system 204 to perform such a process using the example process described in the discussion of Figures 5 to 7

[0034] As discussed above, the computing device 128 includes one or more processors 152 configured to execute instructions, applications, or programs stored in a memory 154 accessible to the one or more processors. In some examples, the one or more processors 152 can include hardware processors, including but not limited to hardware central processing units (CPUs), graphics processing units (GPUs), and the like. While in many cases these techniques are described herein as being performed by the one or more processors 152, in some cases these techniques can be implemented by one or more hardware logic components, such as field-programmable gate arrays (FPGAs), complex programmable logic devices (CPLDs), application-specific integrated circuits (ASICs), 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 computer-readable media. Computer-readable media can include both computer storage media and communication media including any medium that facilitates transfer of a computer program from one place to another. A storage media can be any available media that can be accessed by a general purpose or special purpose computing device. By way of example, and not limitation, such computer-readable media can comprise RAM, ROM, EEPROM, FLASH memory, CD-ROM or other optical disk storage, magnetic disk storage or other magnetic storage devices, or any other storage medium that can be used to carry or store desired program code means in the form of computer-executable instructions, data structures, or program modules and

[0036] Those skilled in the art will further appreciate that items or portions thereof can be transferred between computer 128 and other devices, for example, in the form of computer-executable instructions or data structures implemented to carry out the various functions and operations described herein. Additionally, a mobile computing device can be configured to function as a server or a client of multiple devices, including by operating as a server or a client of one or more devices described herein. Some or all of the software components can be executed in a locally-attached memory of another device and communicated with the computing device 128, for example, for purposes of memory management and data integrity. Alternatively, in other implementations some or all of the software components can be executed in a memory on another device and communicated with the computing device 128. Some or all of the system components or data structures can also be stored (e.g., as instructions or structured data) on a non-transitory computer-accessible medium or a portable article to be read 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 can be transmitted to the computing device 128 via a transmission medium or signal, such as an electrical, electromagnetic, or digital signal, carried by a communication medium, such as a wireless link. Various implementations can further include receiving, sending or storing instructions and / or data implemented as program modules to be executed on the computing device 128 as described above. In some embodiments, the system can include one or more servers, which can be implemented as one or more computing devices, and which can be in communication with one or more client devices, such as the computing device 128. The servers can be configured to provide various services to the client devices, such as the computing device 128, including by providing access to various data and / or services, such as the data and / or services described herein. The servers can be configured to provide the various services to the client devices via one or more networks, such as the Internet, a local area network, a wide area network, a metropolitan area network, a wireless network, a data center network, a storage area network, a Fibre Channel network, or any other such network or combination thereof. The servers can be configured to provide the various services to the client devices via one or more communication protocols, such as the Transmission Control Protocol / Internet Protocol (TCP / IP), the User Datagram Protocol (UDP), the File Transfer Protocol (FTP), the Hypertext Transfer Protocol (HTTP), the Simple Mail Transfer Protocol (SMTP), the Simple Object Access Protocol (SOAP), the Remote Procedure Call (RPC) protocol, the Constrained Application Protocol (CoAP), or any other such protocol or combination thereof.

[0037] Figure 2 and Figure 5The computer executable instructions can include, for example, instructions for implementing the steps, functions, and procedures described in this disclosure. The computer executable instructions can also include instructions for implementing various aspects of the disclosure such as the methods, algorithms, functions, procedures, techniques, operations, and other processes disclosed in this disclosure. The computer executable instructions can be stored on a computer readable storage medium, such as the memory 130, and can be executed by the one or more processors 120. The computer executable instructions can be prepared by compiling, or otherwise, translating a computer program written in one or more programming languages, such as C, C++, Java, Visual Basic, or any other programming language. The computer executable instructions can be prepared by translating the computer program into machine language code, assembly language code, bytecode, or any other executable code. The computer executable instructions can be prepared by compiling, or otherwise, translating a computer program written in one or more programming languages, such as C, C++, Java, Visual Basic, or any other programming language. The computer executable instructions can be prepared by translating the computer program into machine language code, assembly language code, bytecode, or any other executable code. The computer executable instructions can be prepared by compiling, or otherwise, translating a computer program written in one or more programming languages, such as C, C++, Java, Visual Basic, or any other programming language. The computer executable instructions can be prepared by translating the computer program into machine language code, assembly language code, bytecode, or any other executable code.

[0038] In particular Figure 2 is a flowchart of an example process 200 for performing sample extraction and protective cover placement for high reactivity materials within a charged particle microscope system. The process 200 can be implemented in the example charged particle microscope apparatus 100 and / or by the computing architecture 150 described above, or in other environments and architectures.

[0039] At 202, a sample can optionally be prepared. For example, the sample can be pre-processed to expose a region of interest to be imaged and / or studied. In some embodiments, this can include a process of forming a sample from a larger specimen, such as a sample extraction procedure in which a portion of the sample is 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 specimen, and the sample manipulator and / or specimen are transferred so that the block is moved away from the body of the specimen. Alternatively or in addition, a 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 specimen can correspond to a battery or a portion of a battery, and the sample can be a portion 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 a support structure. In particular, the nested void is prepared in the support structure by removing a volume of material from the support structure to create a volume that can accommodate at least a portion of the sample. 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, pocket, 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 a beveled edge (e.g., a 45 degree bevel), and the nested void can be a portion of the sample holder proximate to the beveled edge that is milled away using a focused ion beam. Such a nested void can be milled so that at least a portion of the beveled holder extends beyond the sample when the sample is inserted in 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 structure that allows a sample to be imaged / studied when attached thereto. The support structure can be composed, at least in part, of a number of 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 transferred 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 transferred, angled, and / or rotated such that at least a portion of the sample is contained within the nested void. That is, the sample is positioned such that the portion of the sample is located in a volume in which the portion of the support structure that was milled away was located.

[0043] At 208, portions of the support structure are milled away. In particular, portions of the support structure that are proximate to the sample and / or that define the nested void are milled away from the support structure. In some embodiments, edges / surfaces of the support structure that define the nested void are milled away along a 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 that each partially define the nested void along one or more surfaces of the nested void. The multiple different portions of the support structure can be milled such that, between the milled portions, protrusions of the support structure remain proximate to the sample.

[0044] At 210, the milled away material is allowed to re-deposit to form an adhesive bond between the sample and the support structure. As portions of the support structure are 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 unmilled portions of the support structure and / or the sample. In this manner, the milled away material is allowed to form deposits that interconnect to form an adhesive bond between the support structure and the sample. In this manner, by allowing the milled away material to re-deposit, one or more adhesive bonds can be created between the sample and the unmilled portions of the support structure that hold the sample in place. These adhesive bonds are not only easy for a user to create / easy for automation, because these adhesive bonds are created without the introduction of a precursor gas or liquid, this process 200 can be used to attach samples composed of highly reactive materials to a support structure.

[0045] At 212, the sample may optionally be processed to prepare it for imaging and / or study. For example, a portion of the sample may be ground away using a charged particle beam to expose a region of interest in the sample, polished to remove damage from the sample surface, or a combination thereof. In some embodiments, after the exposed surface has been imaged / studied, the sample may be processed one or more additional times, such that different regions of interest are exposed for imaging / study. In some embodiments, when the sample is ground in step 212, the charged particle beam is angled such that the charged particle beam first grinds through a portion of the support structure before it begins to remove a portion of the sample. In this way, this portion of the support structure can act as a protective cap to prevent occlusion on the exposed sample surface. Thus, in addition to creating an adhesion bond without introducing a precursor gas, process 200 may also allow the use of a protective cap without introducing a precursor gas. In some embodiments, processing the sample may include grinding away the adhesion bond between the sample and the sample manipulator, such that the sample is detached from the sample manipulator. In other embodiments, processing the sample may include grinding away a portion of the sample probe, such that the tip of the sample probe remains attached to the sample, and the remaining portion of the sample probe is detached from the sample.

[0046] At step 214, the sample is imaged and / or studied. In various embodiments, the imaging and / or study of the sample corresponds to performing one or more of the following: a series of tomographic scans of the region of interest on the sample, enhanced insertable backscatter detector (CBS) analysis of the region of interest, and electron backscatter diffraction (EBSD) analysis of the region of interest. Steps 212 and 214 can be repeated, allowing imaging and / or study of multiple regions of interest within the sample.

[0047] Figure 3 and Figure 7 This is a visual flowchart illustrating an example process for performing sample extraction and protective cap placement on a highly reactive material according to the present invention. Specifically, Figure 3 It shows the demonstration of the information about Figure 2 The example process 200 described in the commentary executes a series of captured images 300.

[0048] Image 302 illustrates the optional creation of sample 320 from sample body 322. Specifically, image 302 shows a state in which one or more volumes 324 of sample body 322 surrounding sample 320 are ground away using a beam of charged particles (e.g., an ion beam). Image 304 shows a subsequent state in which sample manipulator 326 is attached to sample 320 in an example process. For example, sample 320 can be created using a deposition gas or by combining... Figure 5The described attachment process attaches to the sample manipulator 326. Once the sample 320 is attached to the sample manipulator 326, the last portion 328 of the sample that was previously connected to the sample body is ablated away. Once the sample 320 is completely detached from the sample body in this manner, the sample manipulator 326 can transfer the sample 320 away from the sample body 322.

[0049] Image 306 shows a state in which nested voids 330 are prepared in the support structure 332. For example, a charged particle beam can be used to ablate away material from the support structure 332. The nested voids 330 can correspond to holes, pockets, cavities, or insertion volumes into which a portion of the sample can be inserted. Although not shown in image 306, in some embodiments, the nested voids can correspond to areas that are adjacent and / or abutting raised structures / portions of the support structure, such that when the sample is transferred into the nested voids, a portion of the sample is adjacent and / or abutting the raised structures / portions 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 structure that allows a sample to be imaged / studied when attached thereto. The support structure can be at least partially composed of a number of different materials, including but not limited to silicon, aluminum, copper, etc.

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

[0051] Image 310 shows a state of image 308 in which a plurality of ablation locations 334 have been mapped thereon. In particular, image 310 shows a plurality of ablation locations 334 that each correspond to a portion of the support structure 332 that is to be ablated using a charged particle beam. Image 312 shows a state of the process after the portions 334 of the sample holder 332 have been ablated away and the ablated material is allowed to re-deposit to form an attachment bond 336 between the sample 320 and the support structure 332.

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

[0053] Additionally, the processes described herein in some embodiments have been shown to preserve the crystallinity of high reactivity materials, as evidenced by the acquired Kikuchi patterns of portions of such clean surfaces 408. Figure 4B An image 420 is shown 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 Also shown is the use 428 to help a user process and / or automatically process and study regions of interest in the sample 422.

[0054] Figure 4C Results of sample extraction and protective cap placement on high reactivity materials using prior art techniques are shown. As can be seen, when an attachment 432 is formed between a high reactivity sample 434 and a support structure 436, the sample 434 suffers significant damage. This damage occurs at two separate steps of the prior art system. First, the sample 434 can be damaged due to reactions with external materials (e.g., deposition gas, bonding liquid) that are introduced to form the attachment. Second, even if the damage in this introduction of external materials is not catastrophic, reactions between the external materials and the high reactivity material 434 can cause the surface of the sample 434 to have subsequent catastrophic reactions when illuminated with a charged particle beam. As shown in image 430, due to these reactions, the prior art for in-situ attachment of samples is not suitable for high reactivity materials.

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

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

[0057] Alternatively, in some embodiments of the method, rather than performing step 502, the sample manipulator includes a probe composed of a high-sputtering-rate material (e.g., purchased with such a coating, or purchased without the addition of a coating through in-situ or ex-situ deposition).

[0058] At 504, the sample is brought into proximity to the sample manipulator. In particular, the sample and / or the sample manipulator can be moved such that portions of the sample manipulator that are to be attached to the sample (e.g., a probe, an intermediate body made of a high-sputtering-rate material attached in step 502, etc.) are within 10 microns of each other, within 1 micron of each other, or closer. For example, the sample and / or the sample manipulator can be attached to moving components and / or otherwise configured to be translated, angled, and / or rotated.

[0059] At 506, the high-sputtering-rate material is irradiated with a charged particle beam. In particular, the charged particle beam is used to mill away one or more portions of the high-sputtering-rate material while leaving one or more other portions of the high-sputtering-rate material located in proximity to the sample manipulator to remain unmilled. In this way, as some portions of the high-sputtering-rate material proximate to the sample are removed, there remains a residual portion of the material that is still within 10 microns, 1 micron, or closer to the sample. For example, three portions located on an edge / surface of the high-sputtering-rate material can be milled away, while two portions of the material located between the three portions can remain unmilled.

[0060] At 508, the abraded high-sputter-rate material is allowed to re-deposit to form an adhesive bond between the sample and the sample manipulator. While portions of the high-sputter-rate material are abraded at step 506, the sample is held in a constant position immediately thereafter such that the abraded material is allowed to settle on the un-abraded portions of the high-sputter-rate material and / or the sample. In this manner, the abraded material forms deposits that interconnect to form an adhesive bond between the high-sputter-rate material and the sample. By allowing the abraded material to re-deposit, one or more adhesive bonds can be created between the sample and the un-abraded portions of the high-sputter-rate material that hold the sample in place. These adhesive bonds are not only easy for a user to create / easy to automate because they are created without the introduction of a precursor gas or liquid, this process 500 can be used to adhere samples made of high-reactivity materials to support structures. Moreover, this process 500 allows adhesive bonds to be performed at cryogenic temperatures and / or in a vacuum without the need to develop specialized microscope mechanisms or include a charged-particle system and without the user needing to learn a complex process.

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

[0062] Figure 6A FIG. C illustrates different example embodiments of creating an adhesive between a sample manipulator and a sample within a charged-particle system. For example, Figure 6A An example 610 is depicted in which a sample 612 is adhered to a sample manipulator 614 that corresponds to a sample probe made of a high-sputter-rate material. In this manner, as portions 616 of the sample probe proximate to the sample 612 are abraded, the abraded material at least partially re-deposits to form an adhesive structure 618 between the sample 612 and the sample manipulator 614.

[0063] Figure 6B An example 640 is depicted in which a sample 642 is adhered to a sample manipulator that corresponds to a sample probe 644 coated with a high-sputter-rate material 646. In this manner, as portions 648 of the coating proximate to the sample 642 are abraded, the abraded material at least partially re-deposits to form an adhesive structure 650 between the sample 642 and the sample manipulator. Figure 6C An example 660 is depicted in which a sample 662 is adhered to a sample manipulator that corresponds to a sample probe 664 adhered to an intermediate body 666 made of a high-sputter-rate material. As portions 668 of the intermediate body 666 proximate to the sample 642 are abraded, at least some of the abraded material re-deposits to form an adhesive structure 670 between the sample 662 and the intermediate body 666.

[0064] Figure 7 A series of images 700 are shown demonstrating example performance of an example process for sample extraction and protective cap placement for highly reactive materials using a sample holder with a beveled edge. Image 702 shows an example sample holder 720 with a beveled edge 722. According to the present disclosure, 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, proximate to 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, pocket, or embedded volume into which a portion of a sample can be inserted is created.

[0065] Image 706 shows the sample 726 in the process of being transferred with a sample manipulator 728 such that at least a portion of the sample 726 is positioned within the nested void 724. In particular, 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 rate material, as shown and described in connection with Figure 5 and Figure 6C Image 708 shows a state after the sample 726 has been transferred such that a portion is positioned within the nested void 724 and then the sample 726 is attached to the sample holder 720 by milling away portions of the sample holder 732 proximate to the sample such that the milled away material re-deposits, 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 extending along a 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 a surface of interest 740. In this way, the thin portion of the sample holder 734 acts as a protective cap through which the charged particle beam 736 is first incident, thereby reducing a shadowing effect on the surface of interest 740. In some embodiments, the surface of interest 740 can then be optionally imaged or otherwise investigated using an electron beam 742.

[0067] Examples in accordance with the inventive subject matter of the present disclosure are described in the following enumerated paragraphs.

[0068] A1. A method for sample extraction and protective cap placement of a high reactivity material within a charged particle microscope system, the method comprising: preparing a nested void in a support structure; transferring 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 re-deposits to form an adhesive bond between the sample and a 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, wherein the volume is 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 transferring at least a portion of the sample into the nested void corresponds to transferring the sample such that at least a portion of the sample is inside the hole.

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

[0072] A2.3. The method according to any 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 of paragraphs A1 to A2.3, wherein the method further comprises performing one or more of: 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 of paragraphs A3.1 to A3.1.1, wherein at least a portion of the support structure is used 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 a portion of the support structure as a protective cap comprises positioning the focused ion beam such that a portion of the support structure is milled away before a portion of the sample is milled away by the focused ion beam.

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

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

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

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

[0082] A3.1.5. The method of any of paragraphs A3.1 through A3.1.4, wherein the process further comprises 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 of any of paragraphs A3.1 through A3.1.5, wherein the portion of the sample is milled away at least in part using a swing-mill.

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

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

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

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

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

[0089] A8. The method of any of paragraphs A1 through A3.1.6, wherein the support structure is composed of an inert material that is non-reactive to a focused ion beam.

[0090] A9. The method of any of paragraphs A1 through A3.1.6, wherein the support structure is a tilted holder having a tilted edge.

[0091] A9.1. The method of paragraph A9, wherein at least a portion of the bevel holder extends beyond the sample when the sample is inserted into the nest void.

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

[0093] A9.3. The method of any of paragraphs A9 through A9.2, wherein the beveled edge is ground at a 45 degree angle.

[0094] A9.4. The method of any of paragraphs A9 through A9.3, wherein you can create the beveled edge, or it can be a commercially purchased artifact.

[0095] A10. The method of any of paragraphs A1 through A9.4, wherein the sample is attached to the sample probe by an attachment bond, and wherein transferring at least a portion of the sample into the nest void comprises transferring the sample probe such that at least a portion of the sample is transferred into the nest void.

[0096] A10.1. The method of paragraph A10, further comprising grinding away the attachment bond such that the sample is detached from the sample probe.

[0097] A10.2. The method of paragraph A10, further comprising grinding away a portion of the sample probe such that a tip of the sample probe remains attached to the sample and a remaining portion of the sample probe is detached from the sample.

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

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

[0100] A11.1.1. The method of paragraph A11.1, wherein preparing the sample from the specimen further comprises transferring the sample probe such that the region of interest is distanced from the specimen.

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

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

[0103] A12. The method of any of paragraphs Al to A11.1.3, wherein the sample corresponds to a battery or a portion of a battery.

[0104] A12.1. The method of paragraph A12, wherein the sample 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 of any of paragraphs Al 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 of any of paragraphs Al to A13, wherein the milling is performed with one of a focused ion beam and an electron beam.

[0107] A14.1. The method of 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 so that it is proximate to the sample, wherein a portion of the sample manipulator that is proximate to the sample is comprised of a high sputtering rate material; and milling the high sputtering rate material with a charged particle beam so that a portion of the high sputtering rate material is removed from the sample manipulator, and wherein at least some of the removed high sputtering rate material re-deposits to form an attachment between the sample manipulator and the sample.

[0109] B1.1. The method of paragraph Bl, wherein the high sputtering rate material corresponds to a material that produces a greater number of atoms per ion than silicon or tungsten when irradiated with a particular ion species and voltage.

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

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

[0112] B1.2. The method of any of paragraphs Bl to B1.1.1.1, wherein the high sputtering rate material is copper or brass.

[0113] B2. The method of any of paragraphs Bl to B1.2, wherein translating the sample manipulator comprises translating the sample manipulator so that the portion comprised of the high sputtering rate material is within 10 microns.

[0114] B2.1. The method of paragraph B2, wherein the transfer sample manipulator comprises the transfer sample manipulator such that the portion comprised of the high sputtering rate material is within one micron.

[0115] B3. The method of any of paragraphs B1-B2.1, wherein the sample manipulator comprises a probe comprised of the high sputtering rate material.

[0116] B4. The method of any of paragraphs B1-B2.1, wherein the sample manipulator comprises a probe coated with the high sputtering rate material.

[0117] B4.1. The method of paragraph B4, wherein irradiating the high sputtering rate material comprises abrading away portions of the coating proximate the sample.

[0118] B5. The method of any of paragraphs B1-B2.1, wherein the sample manipulator comprises an intermediate body attached to the probe, and wherein the intermediate body is comprised of the high sputtering rate material.

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

[0120] B5.1.1. The method of 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 of paragraph B5.1, wherein the intermediate body is attached to the probe portion of the sample manipulator by a process comprising:

[0122] transferring the probe portion such that it is proximate the intermediate body; and

[0123] abrading portions of the intermediate body proximate the probe with a charged particle beam, and wherein 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 of any of paragraphs B1-B5.1.2, wherein the charged particle beam is a focused ion beam.

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

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

[0127] B8. The method of any of paragraphs B1-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 a conventional attachment method.

[0128] B9. The method of any of paragraphs Bl 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 of any of paragraphs B8 or B9, wherein the precursor gas comprises platinum.

[0130] B11. The method of any of paragraphs Bl to B10, wherein the method is performed at cryogenic temperatures in a charged particle system.

[0131] B12. The method of any of paragraphs Bl to Bll, wherein the method is performed under vacuum in a charged particle system.

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

[0133] B14. The method of any of paragraphs Bl to B13, wherein milling the high-sputter-rate material comprises milling a plurality of locations on the high-sputter-rate material proximate to the sample.

[0134] B14.1. The method of paragraph B14, wherein each of the plurality of locations is at an edge of the high-sputter-rate material proximate to the sample.

[0135] B14.2. The method of any of paragraphs B14 to B14.1, wherein between the plurality of locations is at least one region of the high-sputter-rate material proximate to the edge of the sample that is not milled away.

[0136] B14.2.1. The method of paragraph B14.2, wherein at least some of the removed high-sputter-rate material is redeposited to form an attachment between the sample and the at least one region of the high-sputter-rate material proximate to the edge of the sample that is not milled away.

[0137] B14.2.2. The method of any of paragraphs B14.2 to B14.2.1, wherein there are a plurality of regions of the high-sputter-rate material proximate to the edge of the sample that are not milled away.

[0138] B14.2.2.1. The method of paragraph B14.2.2, wherein at least some of the removed high-sputter-rate material is redeposited to form an attachment between the sample and a plurality of the at least one region of the high-sputter-rate material proximate to the edge of the sample that is not milled away.

[0139] B14.2.2.2. The method of any of paragraphs B14.2.2 to B14.2.2.1, wherein at least some of the removed high-sputter-rate material is redeposited to form a plurality of attachments between the sample and the high-sputter-rate material.

[0140] B14.2.2.2.1. The method of paragraph B14.2.2.2, wherein each of the plurality of attachments connects the sample to a corresponding one of the at least one region of high sputter rate material along the edge of the sample that was not milled away.

[0141] B14.2.2.2.2. The method of any of paragraphs B14.2.2.2 to B14.2.2.2.1, wherein the plurality is in the at least one region of high sputter rate material along the edge of the sample that was not milled away.

[0142] B14.2.2.2.2.1. The method of paragraph B14.2.2.2.2, wherein at least four attachments are formed between the sample and corresponding regions of high sputter rate material along the edge of the sample that was not milled away.

[0143] C1. A charged particle system, the system comprising: a charged particle emitter configured to emit charged particles toward 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 resulting from illumination by the charged particles; one or more processors; and a memory storing non-transitory computer-readable instructions that, when executed by the one or more processors, cause the one or more processors to perform a method according to any of paragraphs Al to A14.1 and / or Bl to B14.2.2.2.2.1.

[0144] C2. The charged particle system of paragraph C1, further comprising a vacuum chamber comprising the sample.

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

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

[0147] C3. The charged particle system of any of paragraphs Cl to C2.2, wherein the instructions cause the one or more processors to perform a method according to any of paragraphs Al to A14.1 and / or Bl to B14.2.2.2.2.1 while the sample is at a cryogenic temperature.

[0148] D1. Use of the system according to any of paragraphs C1 to C3 for carrying out the method according to any 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 that, when executed by a processor, cause the processor to start carrying out the method according to any of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

[0150] F1. Use of the non-transitory computer readable medium of paragraph E1 for carrying out the method according to any of paragraphs A1 to A12.7 and / or B1 to B14.2.2.2.2.1.

Claims

1. A method for performing sample extraction and protective cover placement within a charged particle microscope system, the method comprising: preparing a nested void in a support structure, wherein preparing the nested void comprises milling away a volume of the support structure; transferring 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 adhesive bond between the sample and a remaining portion of the support structure.

2. The method of claim 1, wherein transferring the at least a portion of the sample into the nested void corresponds to transferring the sample such that the at least a portion of the sample is within the volume.

3. The method of claim 2, wherein the nested void is configured such that when the adhesive bond is formed between the sample and the support structure, the at least a portion of the sample is positioned at a location where the volume of the sample is milled away.

4. The method of claim 1, wherein the method further comprises the steps of: milling away a portion of the sample to expose a surface of interest; and imaging at least a portion of the surface of interest.

5. The method of claim 4, wherein at least a portion of the support structure is used as a protective cover during milling of the sample.

6. The method of claim 5, wherein using the portion of the support structure as a protective cover comprises positioning a 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.

7. The method of claim 1, wherein the support structure is one of a sample grid, a sample holder, and an aluminum block.

8. The method of claim 7, wherein the support structure is composed of an inert material that is not chemically reactive to a focused ion beam.

9. The method of claim 1, wherein the support structure is a tilted holder having a tilted edge, and wherein the nested void is prepared proximate to the tilted edge.

10. The method of claim 9, wherein at least a portion of the tilted holder extends beyond the sample when the sample is inserted into the nested void.

11. The method of claim 9, further comprising using the tilted edge as a protective cover by first milling through the tilted holder to mill away a section of the sample.

12. The method of claim 1, wherein the sample is attached to a sample probe by an adhesive bond, and wherein transferring at least a portion of the sample into the nested void comprises transferring the sample probe such that the at least a portion of the sample is transferred into the nested void.

13. The method of claim 12, wherein attaching the sample probe to the sample comprises the steps of: transferring the sample probe such that it is proximate to the sample, wherein a portion of the sample probe that is proximate to the sample is composed of a high sputter rate material; and transferring the sample probe such that it is proximate to the sample, wherein a portion of the sample probe that is proximate to the sample is composed of a high sputter rate material; and ​ ablation of the sample probe and the sample.

14. The method of claim 13, wherein the sample probe comprises one of: a probe composed of the high sputtering rate material; a probe coated with the high sputtering rate material; and an intermediate body attached to a probe.

15. The method of claim 1, wherein the sample corresponds to a battery or a portion of a battery.

16. A charged particle system, the system comprising: a charged particle emitter configured to emit charged particles toward 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 due to illumination by the charged particles; one or more processors; and a memory storing non-transitory computer-readable instructions that, when executed by the one or more processors, cause the one or more processors to perform the steps of: preparing a nested void in a support structure, wherein preparing the nested void comprises abrading away a volume of the support structure; transferring at least a portion of a sample into the nested void; and abrading material from a region of the support structure that defines the nested void, such that at least some of the material abraded from the support structure re-deposits to form an adhesive bond between the sample and a remaining portion of the support structure.

17. The charged particle system of claim 16, wherein the nested void is configured such that, when the adhesive bond is formed between the sample and the support structure, the at least a portion of the sample is positioned at a location where the volume of the sample was abraded away.

18. The charged particle system of claim 16, further comprising a vacuum chamber containing a sample, and wherein the instructions cause the one or more processors to perform the steps while the sample is in a vacuum state.

19. The charged particle system of claim 16, wherein the instructions cause the one or more processors to perform the steps while the sample is at a cryogenic temperature.

20. A non-transitory computer-readable medium storing instructions that, when executed by a processor, cause the processor to initiate performance of the steps of: preparing a nested void in a support structure, wherein preparing the nested void comprises abrading away a volume of the support structure; transferring at least a portion of a sample into the nested void; and abrading material from a region of the support structure that defines the nested void, such that at least some of the material abraded from the support structure re-deposits to form an adhesive bond between the sample and a remaining portion of the support structure. ​ ​ ​

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