Systems and methods for performing sample lift-out of highly reactive materials

Abstract

To perform a sample lift-out of a highly responsive material in a charge particle microscope system and a protection cap arrangement.SOLUTION: A method includes: preparing a nested gap in a support structure; moving forward at least a part of a sample into the nested gap side by side; and milling a material from the region of the support structure that defines the nested gap. The material from the region of the support structure is milled so that at least a part of the removed material is re-deposited and an attachment binding unit is formed between the sample and the remaining part of the support structure. In various different embodiments, the sample can be examined by at least one of continuous sectioning laminagraphy for the sample, an expanded insertable backscattering detector (CBS) analysis for the sample, and an electronic backscattering diffraction for the sample (EBSD).SELECTED DRAWING: Figure 1

Description

[Background technology]

[0001] In scanning charged particle microscopes and transmission charged particle microscopes, a charged particle beam is used to image or otherwise interrogate an area of ​​interest on a sample. Often, before the area of ​​interest can be imaged and / or interrogated, it is necessary to prepare and / or manipulate the sample within the system to allow the area of ​​interest to be exposed or otherwise prepared. In current systems, such preparation often includes one or more of the following: preparing the sample from a larger specimen using a charged particle beam; mounting the sample on a manipulation probe to allow the sample to be translated within the microscope system; and mounting the sample on a sample holder so that the area of ​​interest on the sample can be processed, imaged, and / or otherwise interrogated.

[0002] In current systems, the sample is attached to the probe and / or sample holder using a precursor gas or a pooled liquid. Specifically, in some attachment methods, a precursor gas is introduced into the volume surrounding the sample, where the gas molecules form deposits on the sample, probe, and / or sample holder when irradiated with a charged particle beam. In other current attachment methods, a liquid is first introduced to the sample, probe, and / or sample holder, and the liquid is irradiated with a charged particle beam so that the liquid hardens, forming an attachment bond between the sample and the probe and / or sample holder. However, while these systems are effective for many common applications, they each suffer from drawbacks that make them unsuitable for some microscopic investigations.

[0003] For example, charged particle microscope systems investigate samples in sealed chambers for reducing contamination of optical components, reducing the effect of undesired particles on the charged particle beam, and having unwanted deposits on the sample. The introduction of precursor gases and / or liquids adds additional material to the chamber of the charged particle microscope system, increasing these undesired effects. In addition, the introduction of gases or liquids requires specially adapted 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 gases may cause degradation of the sample surface and / or make the sample more reactive to the charged particle beam if subsequent post-mounting milling or imaging is performed. Thus, there is a need for new mounting and sample handling systems and processes that allow imaging and investigation of highly reactive materials. Summary of the Invention

[0004] Disclosed herein are methods and systems for performing sample lift-out and protective cap placement of highly reactive materials within a charged particle microscope system. The method includes preparing a nested cavity in a support structure, translating at least a portion of the sample into the nested cavity, and milling material from a region of the support structure that defines the nested cavity. The material from the region of the support structure is milled such that at least a portion of the removed material is redeposited to form an attachment bond between the sample and the remaining portion of the support structure. In various embodiments, the sample may then be investigated using one or more of serial sectioning tomography on the sample, extended insertable backscatter detector (CBS) analysis on the sample, and electron backscatter diffraction (EBSD) analysis on the sample.

[0005] A system for performing sample lift-out and protective cap placement of highly reactive materials in a charged particle system according to the present disclosure may include a charged particle emitter configured to emit charged particles toward the sample, a sample holder configured to support the sample, an optical column configured to direct the charged particles incident on the sample, and a detector system configured to detect emissions from the sample due to irradiation by the charged particles. 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 prepare a nested cavity in a support structure, translate at least a portion of the sample into the nested cavity, and mill material from a region of the support structure that defines the nested cavity. [Brief description of the drawings]

[0006] The detailed description will now be described with reference to the accompanying drawings, in which the left-most digit(s) of a reference number identifies the figure in which the reference number first appears. The same reference numbers in different figures indicate similar or identical items.

[0007] [Figure 1] 1 illustrates an exemplary system for performing sample lift-out and protective cap placement of highly reactive materials and / or for creating a mount between a sample manipulator and a sample in a charged particle microscope system. [Diagram 2] FIG. 1 is a flow diagram of an illustrative process for performing sample lift-out and protective cap placement of highly reactive materials in a charged particle microscope system. [Diagram 3] 1 is a series of captured images illustrating an exemplary implementation for performing sample lift-out and protective cap placement of highly reactive materials within a charged particle microscope system. [Figure 4A] 13A-13C are captured images showing exemplary results of highly reactive material sample lift-out and protective cap placement according to the present disclosure. [Figure 4B]13A-13C are captured images showing exemplary results of highly reactive material sample lift-out and protective cap placement according to the present disclosure. [Figure 4C] 13A-13C are captured images showing exemplary results of highly reactive material sample lift-out and protective cap placement according to the present disclosure. [Diagram 5] 1 illustrates a flow diagram of an illustrative process for creating a mounting between a sample manipulator and a sample in a charged particle system. [Figure 6A] 1 illustrates an exemplary embodiment for creating a mounting between a sample manipulator and a sample in a charged particle system. [Figure 6B] 1 illustrates an exemplary embodiment for creating a mounting between a sample manipulator and a sample in a charged particle system. [Figure 6C] 1 illustrates an exemplary embodiment for creating a mounting between a sample manipulator and a sample in a charged particle system. [Figure 7] 1 shows a series of images illustrating an exemplary implementation of an exemplary process for sample lift-out and protective cap placement of highly reactive materials using a sample holder with a beveled edge.

[0008] Like reference numbers refer to corresponding parts throughout the several views of the drawings. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0009] Methods and systems are disclosed for performing sample lift-out and protective cap placement of highly reactive materials in a charged particle microscope system. More specifically, the disclosure includes methods and systems in which a nested cavity is created in a support structure, the sample is translated such that at least a portion of the sample is located within the nested cavity, and then material from the region of the support structure that defines the nested cavity is milled away. The material from the region of the support structure is located proximate to the sample such that at least a portion of the removed material redeposits to form one or more attachment joints between the sample and the remaining portion of the support structure. In this manner, the sample can be attached to a sample holder without the need to add precursor gas or other types of attachment media to the charged particle system. In addition, because the attachment is formed by passive redeposition of the milled material, the likelihood of reaction and / or other types of damage to the sample is much less. 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 has been mounted in the sample holder in this manner, one or more regions of interest of the sample can be imaged and / or investigated using one or more methodologies, such as, but not limited to, serial sectioning tomography of the sample, enhanced insertable backscatter detector (CBS) analysis of the sample, and electron backscatter diffraction (EBSD) analysis of the sample.

[0010] Additionally, methods and systems for creating an attachment between a sample manipulator and a sample in a charged particle system are also disclosed herein. Specifically, the present disclosure includes methods and systems for attaching a sample to a holder or manipulator by irradiation of a high sputter yield material proximate to the sample. First, the sample manipulator is translated so that a portion of the manipulator made of the high sputter yield material is located proximate (e.g., within microns) to the sample. Then, an area of ​​the high sputter yield material proximate to the sample is milled away using a charged particle beam, whereby at least a portion of the removed high sputter yield material is redeposited to form an attachment between the sample manipulator and the sample. According to the present disclosure, a high sputter yield material corresponds to a material that, when irradiated with a particular ion beam species and voltage, produces a greater number of atoms / ions than silicon or tungsten. For example, a high sputter yield material is defined as a material, such as copper or zinc, that emits greater than 5, 7, 8, or 10 atoms / ion when the material is irradiated with a 30 kV Ga+ focused ion beam.

[0011] Generally, in the figures, elements that are likely to be included in a given example are shown with solid lines, while elements that are optional in a given example are shown with dashed lines, however, elements shown with solid lines are not required for all examples of the present disclosure, and elements shown with solid lines may be omitted from particular examples without departing from the scope of the present disclosure.

[0012] 1 illustrates an exemplary system 100 for performing sample lift-out and protective capping of highly reactive materials and / or for creating an attachment between a sample manipulator and a sample within a charged particle microscope system. Specifically, FIG. 1 shows an exemplary environment 102 including an exemplary microscope system 104 for creating an attachment between a sample manipulator 106 and a sample 108 and / or for performing sample lift-out and protective capping of highly reactive materials in situ. It should be noted that the present disclosure is not limited to environments including microscopes, and that in some embodiments, the environment 100 may include different types of systems configured to manipulate and / or otherwise interrogate the sample 108.

[0013] The exemplary microscope system 104 may be or include one or more of various types of optical microscopes 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 cryogenic compatible microscope, a focused ion beam (FIB) microscope, a dual beam microscope system, or combinations thereof. Figure 1 illustrates the exemplary microscope system 104 as being a dual beam microscope system including a STEM column 110 and a FIB column 112.

[0014] 1 depicts the exemplary microscope system 104 as including a STEM column 110 for irradiating a sample 108 with a charged particle beam 114. The STEM column 110 includes an electron source 116 (e.g., a thermionic electron source, a Schottky emitter source, a field emitter source, etc.) that emits the electron beam 114 toward the sample 108 along an electron emission axis 118. 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 through the sample 108. Although FIG. 1 depicts the exemplary microscope system 104 as including the 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.

[0015] The acceleration lens 120 accelerates / decels, focuses, and / or directs the electron beam 114 towards the electron focusing column 122. The electron focusing column 122 focuses the electron beam 114 so that it is incident on at least a portion of the sample 108. In addition, the focusing column 122 may correct and / or adjust 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 an aperture, a deflector, a transfer lens, a scanning coil, a condenser lens, an objective lens, etc. that focus the electrons from the electron source 116 in unison to a small spot on the sample 108. By adjusting the direction of the electron beam with the deflector and / or the scanning coil, various locations of the sample 108 may be scanned. In this manner, the electron beam 114 may act as an imaging beam that is scanned across the surface of the sample (i.e., the surface of the layer that is proximate to the STEM column 104 and / or illuminated by the electron beam 114). This illumination of the surface of the sample 108 causes the component electrons of the electron beam 114 to interact with the component electrons / molecules / features of the sample, which in turn cause the component electrons / molecules / features to be emitted by the sample 108 as ejections 124. The particular ejections that are emitted are based on the corresponding elements / molecules / features that caused them to be emitted, such that the ejections can be analyzed to determine information about the corresponding elements / molecules. Additionally, while FIG. 1 illustrates the ejections 124 as traveling downstream of the sample 108, one skilled in the art will appreciate that the ejections may be emitted in other directions, including, but not limited to, toward the charged particle source 116.

[0016] 1 further illustrates detector systems 126(a) and 126(b) for detecting emissions 124 resulting from the electron beam 114 incident on the sample 108. The detector system 126 may comprise 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 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 may be configured to detect different types of emissions, or different parameters of an emission may be configured to be detected by different detectors and / or different portions. 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.

[0017] 1 also depicts the example microscope system 104 as including 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 may mill away portions of a specimen body to reveal or otherwise prepare the sample 108. In other embodiments, the example microscope system 104 may include other types of delayering components, such as a laser, a mechanical blade (e.g., a diamond blade), an electron beam, etc. The FIB column 112 is depicted as including a charged particle emitter 132 configured to emit a plurality of ions 134 along an ion emission axis 136.

[0018] The ion emission axis 136 is a central axis extending from the charged particle emitter 132 through the sample 108. The FIB column 112 further includes an ion focusing column 138 comprising one or more of an aperture, a deflector, a transfer lens, a scanning coil, a condenser lens, an objective lens, etc., that focus the ions from the charged particle emitter 132 together into a small spot on the sample 108. In this manner, the elements in the ion focusing column 138 may 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, the FIB column 112 may be configured to remove a surface layer of the sample 108 having a known thickness from the sample 108 during image acquisition during slice-and-view imaging.

[0019] 1 illustrates the exemplary microscope system 104 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 a sample 108 and can translate, rotate, and / or tilt the sample 108 relative to the exemplary microscope system 104. For example, the sample holder 140 can include a grid or structure to which a sample or specimen can be attached and / or otherwise held. Additionally, the sample manipulator 108 is a feature in the microscope chamber 130 that can interact with the sample 108 such that the sample can be translated, angled, and / or rotated. For example, FIG. 1 illustrates the sample manipulator as including a probe portion that extends from a body and to which a sample can be attached. The sample loading chamber 142 may be sealable from the microscope chamber 130 and may be capable of retracting the sample holder 140 into the sample loading chamber 142 so that a user can access and / or interact with the sample holder 140 while it is in the sample loading chamber 142.

[0020] The environment 100 is also shown as including one or more computing devices 128. Those skilled in the art will appreciate that the computing devices 128 shown in FIG. 1 are merely exemplary and are not intended to limit the scope of the present disclosure. Computing systems and devices may include any combination of hardware or software capable of performing the specified functions, including computers, network devices, Internet appliances, PDAs, wireless telephones, controllers, oscilloscopes, amplifiers, etc. Computing device 128 may also be connected to other devices not shown, or may alternatively operate as a stand-alone system.

[0021] 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 separate devices from the exemplary microscope system 104 that communicate with the exemplary microscope system 104 via a network communication interface, or may be a combination thereof. For example, the exemplary microscope system 104 may include a first computing device 128 that is a component part of the exemplary microscope system 104 and functions as a controller that drives the operation of the exemplary charged particle microscope system 104 (e.g., adjusting the scan location on the sample by operating a scan coil, etc.). In such an embodiment, the exemplary microscope system 104 may also include a second computing device 128 that is a desktop computer separate from the exemplary microscope system 104 and is executable 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 of the detector data. The computing device 128 may be further configured to accept user selections via a keyboard, mouse, touchpad, touchscreen, etc. The computing device 128 is configured to generate an image of a surface of the sample 108 in the exemplary microscope system 104 based on the data and / or data signals from the detector system 126 .

[0022] Additionally, the computing device 128 is configured to control the FIB column 112, the sample manipulator 106, and / or the sample holder 140 to enable sample lift-out and protective cap placement to be performed on highly reactive materials within the charged particle microscope system 104. For example, the computing device 128 may cause the FIB column 112 to use a plurality of ions 134 to mill a nested cavity into a support structure (e.g., a sample grid, a sample holder, or other structure that allows the sample to be imaged / probed when the sample is attached). One or more user selections, automated programs, or combinations thereof may enable the computing device 128 to translate (e.g., translate, angle, and / or rotate) the sample holder 140 or the sample manipulation device 106 such that at least a portion of the sample 108 is positioned within the nested cavity. Once the sample 108 is positioned at least partially within the nested cavity, the computing device 128 may cause the FIB column 112 to mill away a portion of the support structure near and / or defining a portion of the sample. User selection, an automated program, or a combination thereof, selects a portion of the support structure to be milled away in such a way that the milled material redeposits in the nested cavity to form an attachment bond between the support structure and the portion of the sample 108. In this manner, an interconnect 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 gases or other materials to the microscope chamber 130. In some embodiments, the computing device 128 may be further configured to cause the exemplary microscope system 104 to prepare the sample 108 prior to attachment (e.g., remove the sample from a larger sample body to expose surfaces / structures of interest), process the sample to prepare the sample for imaging / investigation, or perform imaging / investigation of one or more regions of the sample 108.

[0023] Alternatively, or in addition, 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 the need to add additional deposition gases or other materials to the microscope chamber 130. For example, the computing device 128 may cause a high sputter yield material (e.g., copper) to be positioned proximate to the sample 108. The high sputter yield material may optionally be attached to the sample manipulator, which itself may include the high sputter yield material (e.g., purchased with such a coating or purchased without, if a coating is added by in situ or ex situ deposition).

[0024] A user selection, an automated program, 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 proximate the sample while leaving one or more other portions of the high sputter yield material proximate the sample manipulator unmilled. In this manner, some portions of the high sputter yield material near the sample are removed while still leaving portions of the material within 10 microns, within 1 micron, or closer to the sample. Thus, as the milled high sputter yield material is redeposited, one or more attachment joints are formed between the sample and the sample manipulator.

[0025] FIG. 1 further includes a schematic diagram illustrating an exemplary computing architecture 150 of a computing device 128. The exemplary computing architecture 150 illustrates additional details of hardware and software components that may be used to implement the techniques described in this disclosure. Those skilled in the art will appreciate that the computing architecture 150 may be implemented in a single computing device 128 or across multiple computing devices. For example, individual modules and / or data structures depicted in the computing architecture 150 may be executed by and / or stored on different computing devices 128. In this manner, various process steps of the inventive methods disclosed herein may be executed and / or performed by separate computing devices 128 and in various orders within the scope of the present disclosure. In other words, the functionality provided by the illustrated components may be combined into fewer components or distributed among additional components in some implementations. Similarly, in some implementations, the functionality of some of the illustrated components may not be implemented and / or other additional functionality may be available.

[0026] In the exemplary 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. Without intending to be limiting, the exemplary computing architecture 150 is illustrated as including a control module 156 stored in the memory 154. As used herein, the term "module" is intended to represent an exemplary division 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 functions and / or similar functions may be arranged differently (e.g., combined into fewer modules, split into more modules, etc.). Furthermore, while certain functions and modules are described herein as being implemented by software and / or firmware executable on a processor, in other cases, any or all modules may be implemented in whole or in part by hardware (e.g., specialized processing units, etc.) to perform the described functions. As discussed above, in various implementations, the modules described herein in connection with the exemplary computing architecture 150 may be executed across multiple computing devices 128.

[0027] The control module 156 may be executable by the processor 152 to cause the computing device 128 and / or the exemplary microscope system 104 to perform one or more actions and / or system functions or maintenance. In some embodiments, the control module 156 may cause the exemplary microscope system 204 to perform a sample lift-out and / or protective cap placement of a highly reactive material within the charged particle microscope system 104. For example, the control module 156 may cause the exemplary microscope system 204 to perform such a process using the exemplary processes described in the notes for FIGS. 2-4. Alternatively, or in addition, the control module 156 may 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 the need to add additional deposition gases or other materials to the microscope chamber 130. For example, the control module 156 may cause the exemplary microscope system 204 to perform such a process using the exemplary processes described in the notes for FIGS. 5-7.

[0028] As discussed above, computing device 128 includes one or more processors 152 configured to execute instructions, applications, or programs stored in memory 154 accessible to the one or more processors. In some embodiments, one or more processors 152 may include a hardware processor, including, but not limited to, a hardware central processing unit (CPU), a graphics processing unit (GPU), or the like. While in many cases, the techniques are described herein as being performed by one or more processors 152, in some cases, the techniques may 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.

[0029] 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: computer storage media and communication media. Computer storage media can include volatile and non-volatile, removable and fixed media implemented in any method or technology for storage of information such as computer-readable instructions, data structures, program modules, or other data. Computer storage media include, but are not limited to, random access memory (RAM), read-only memory (ROM), erasable programmable read-only (EEPROM), flash memory or other memory technology, compact disc read-only memory (CD-ROM), digital versatile disk (DVD) or other optical storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other non-transmission medium that can be used to store desired information and that can be accessed by a computing device. In general, computer storage media can include computer-executable instructions that, when executed by one or more processing units, cause various functions and / or operations described herein to be performed. 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.

[0030] Those skilled in the art will also recognize that items or portions of items may be transferred between memory 154 and other storage devices for memory management and data integrity purposes. Alternatively, in other implementations, some or all of the software components may execute in memory on another device and communicate with computing device 128. Some or all of the system components or data structures may also be stored in a non-transitory computer-accessible medium or in a portable product read by an appropriate drive (e.g., as instructions or structured data), various examples of which are described above. In some implementations, instructions stored in a computer-accessible medium separate from computing device 128 may be transmitted to computing device 128 via a transmission medium or signal, such as an electrical, electromagnetic, or digital signal carried over a communication medium, such as a wireless link. Various implementations may further include receiving, sending, or storing instructions and / or data implemented in accordance with the preceding description of a computer-accessible medium.

[0031] 2 and 5 are illustrative process flow diagrams shown as a collection of logical flow graph blocks, which represent a sequence of operations that may be implemented in hardware, software, or a combination thereof. In a software context, the blocks represent computer-executable instructions stored on one or more computer-readable storage media that, when executed by one or more processors, perform the recited operations. Generally, computer-executable instructions include routines, programs, objects, components, data structures, etc. that perform particular functions or implement particular abstract data types. The order in which the operations are described should not be construed as a limitation, and any number of the described blocks can be combined in any order and / or in parallel to implement a process.

[0032] 2 is a flow diagram of an illustrative process 200 for performing sample lift-out and protective cap placement of highly reactive materials within a charged particle microscope system. The process 200 may be implemented in the exemplary charged particle microscope setup 100 and / or by the computing architecture 150 described above, or in other environments and architectures.

[0033] At 202, the sample is optionally prepared. For example, the sample may be pre-treated to expose the area of ​​interest to be imaged and / or interrogated. In some embodiments, this may include forming the sample from a larger sample using a process such as a sample lift-out procedure that mills away a portion of the sample to expose a chunk containing the area of ​​interest, where the chunk is attached to a sample manipulator, the chunk is detached from the body of the sample, and the sample manipulator and / or sample is translated so that the chunk is away from the body of the sample. Alternatively, or in addition, the surface of the sample may be milled away and / or polished to expose the area of ​​interest and / or remove damage from the surface to allow for high quality imaging / interrogation. In some embodiments, the sample may correspond to a battery or a portion of a battery, and the sample may be a portion of the sample that includes at least one of lithium, manganese, lithium polymer, lithium cobalt oxide, lithium manganese oxide, lithium manganese cobalt oxide, etc.

[0034] At 204, a nested void is prepared in the support structure. Specifically, 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 material out of the support structure. The nested void can correspond to a hole, pocket, or inset 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 beveled edge), and the nested void can be a portion of the sample holder near the beveled edge that is milled out with a focused ion beam. Such a nested void can be milled such that when a sample is inserted into the nested void, at least a portion of the beveled holder extends beyond the sample.

[0035] In various embodiments, the support structure may correspond to one or more of a sample grid, a sample holder, or other structure that allows for imaging / probing the sample when mounted. The support structure may be at least partially constructed from many different materials, including but not limited to silicon, aluminum, copper, etc. In some embodiments, the support structure is constructed from an inert material that does not react to the charged particle beam.

[0036] At 206, the sample is translated such that at least a portion of the sample is positioned within the nested cavity. For example, the sample may be attached to a movable sample manipulator (e.g., a sample probe) that is translated, angled, and / or rotated such that at least a portion of the sample is contained within the nested cavity. That is, the sample is positioned such that a portion of the sample is located in the volume in which the portion of the support structure that was milled away was located.

[0037] At 208, portions of the support structure are milled away. Specifically, portions of the support structure near portions of the sample and / or defining 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 the depth of the sample. Alternatively, or in addition, multiple portions of the support structure that partially define the nested void may be milled away in this manner. For example, a charged particle beam may be used to mill away multiple distinct portions of the support structure, each of which partially defines the nested void along one or more surfaces of the nested void. Such multiple distinct portions of the support structure may be milled such that between the milled portions, protrusions of the support structure remain in proximity to the sample.

[0038] At 210, the milled material is redeposited to form an attachment bond between the sample and the support structure. While and immediately after portions of the support structure are milled away at step 208, the sample is held in a fixed position to anchor the milled away material onto the support structure and / or the non-milled portions of the sample. In this manner, the milled material is allowed to form interconnecting deposits to form an attachment bond between the support structure and the sample. In this manner, by redepositing the milled material, 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 automated because they are created without the introduction of precursor gases or liquids, but this process 200 can also be used to attach samples composed of highly reactive materials to support structures.

[0039] At 212, the sample is optionally processed to prepare the sample for imaging and / or investigation. For example, portions of the sample may be milled away with a charged particle beam to expose regions of interest in the sample, polished to remove damage from the surface of the sample, or a combination thereof. In some embodiments, after the exposed surface is imaged / investigated, the sample may be further processed one or more times so that various regions of interest are exposed for imaging / investigation. In some embodiments, when the sample is milled at step 212, the charged particle beam is angled such that it first mills through a portion of the support structure before beginning to remove portions of the sample. In this way, a portion of the support structure may be used as a protective cap to prevent curtaining of the exposed sample surface. Thus, in addition to creating an attachment joint without introducing a precursor gas, the process 200 may also allow for the utilization of a protective cap without introducing a precursor gas. In some embodiments, processing the sample may include milling away an attachment joint 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 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 detached from the sample.

[0040] At 214, the sample is imaged and / or interrogated. In various embodiments, the imaging and / or interrogation of the sample corresponds to performing one or more of serial sectioning tomography of a region of interest on the sample, an enhanced insertable backscatter detector (CBS) analysis of the region of interest, and an electron backscatter diffraction (EBSD) analysis of the region of interest. Steps 212 and 214 may be repeated such that multiple regions of interest within the sample may be imaged and / or interrogated.

[0041] 3 and 7 are visual flow diagrams illustrating an exemplary process for performing highly reactive material sample lift-out and protective cap placement according to the present disclosure. Specifically, FIG. 3 shows a series of captured images 300 illustrating an exemplary implementation of the exemplary process 200 described in the notes regarding FIG.

[0042] Image 302 illustrates the optional creation of a sample 320 from a sample body 322. In particular, image 302 illustrates one or more volumes 324 of the sample body 322 surrounding the sample 320 being milled away using a charged particle beam (e.g., an ion beam). Image 304 illustrates a subsequent state of the exemplary process in which a sample manipulator 326 is attached to the sample 320. For example, the sample 320 may be attached to the sample manipulator 326 using a deposition gas or by the attachment process described in connection with FIG. 5. Once the sample 320 is attached to the sample manipulator 326, a final portion 328 of the sample that previously connected the sample to the sample body is milled away. Once the sample 320 is fully separated from the sample body in this manner, the sample manipulator 326 may translate the sample 320 away from the sample body 322.

[0043] Image 306 shows a nested void 330 prepared in support structure 332. For example, a charged particle beam can be used to mill away material from support structure 332. Nested void 330 can correspond to a hole, pocket, cavity, or inset volume into which a portion of a sample can be inserted. Although not shown in image 306, in some embodiments, the nested void can correspond to an area adjacent 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 comes close to and / or abuts the raised structure / portion of the support structure. In various embodiments, support structure 332 can correspond to one or more of a sample grid, a sample holder, or other structure that allows the sample to be imaged / probed when the sample is attached. Support structures can be at least partially constructed from many different materials, including but not limited to silicon, aluminum, copper, and the like.

[0044] Image 308 shows the sample 320 after it has been translated, tilted, rotated, or otherwise manipulated relative to the support structure such that at least a portion of the sample is positioned within the nested cavity 330. The sample is shown attached to a movable sample manipulator 326 (i.e., a sample probe), and the sample has been translated, angled, and / or rotated such that at least a portion of the sample 320 is received within the nested cavity 330.

[0045] Image 310 shows the state of image 308 with multiple milling locations 334 mapped onto image 308. Specifically, image 310 shows multiple milling locations 334, each corresponding to a portion of a 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 the milled material is redeposited to form an attachment bond 336 between the sample 320 and the support structure 332.

[0046] 4A-C are captured images showing exemplary results of sample lift-out and protective cap placement of highly reactive materials according to the present disclosure and according to the prior art. FIG. 4A is an image 410 of the sample 320 from FIG. 3 after further processing of the sample 320 to prepare the sample 320 for imaging and / or investigation. For example, a portion of the sample 320 has been milled away with a charged particle beam to expose a clean surface 412 in a region of interest of the sample, and then polished to remove damage from the surface of the sample. Specifically, FIG. 4A shows an example in which a portion of the sample 320 has been removed and cleaned to expose a clean reactive surface 412(a) (i.e., a clean surface of a portion of the sample composed of reactive material) and a clean stable surface 412(b) (i.e., a clean surface of a portion of the sample composed of non-reactive material). In such embodiments where the sample is composed of both stable and reactive materials, milling through the stable material may be performed first, whereby the stable material acts as a cap to reduce curtaining at the clean reactive surface 412(a). Alternatively, in some embodiments, milling may be performed such that a portion of the support structure 322 is milled through first, whereby the support structure 322 acts as a cap to reduce curtaining at the clean reactive surface 412(a). Using the processes described herein, high quality EBSD maps and / or band contrast maps may be obtained for the clean surface 412 of the highly reactive material that were not previously possible with conventional techniques.

[0047] Additionally, the processes described herein in some embodiments have been shown to maintain the crystallinity of the highly reactive material as evidenced by the Kikuchi patterns obtained on portions of such cleaned surface 408. Figure 4B shows an image 420 in which a sample 422 has been inserted into a nested cavity 424 in a support structure 426 and mounted using techniques according to the present disclosure. Figure 4B further illustrates the use of 428 to assist in user and / or automated processing and investigation of areas of interest in sample 422.

[0048] FIG. 4C shows the result of sample lift-out and protective cap placement of a highly reactive material using the prior art technique. As can be seen, when the attachment 432 was formed between the highly reactive sample 434 and the support structure 436, the sample 434 was severely damaged. This damage occurs in two separate steps in the prior art system. First, the sample 434 can be damaged by reaction with the foreign material (e.g., deposition gas, binding liquid) introduced to form the attachment. Second, even if the damage from the introduction of such foreign material is not catastrophic, the reaction between the foreign material and the highly reactive material 434 when irradiated with a charged particle beam can cause subsequent catastrophic reactions of the surface of the sample 434. As shown in image 430, due to these reactions, the prior art techniques for in situ attachment of samples are not effective for highly reactive materials.

[0049] 5 is a flow diagram of an illustrative process 500 for creating an attachment between a sample manipulator and a sample in a charged particle system. The process 500 may be implemented in the exemplary processes 200-400, the exemplary charged particle microscope setup 100, and / or by the computing architecture 150 described above, or in other environments and architectures.

[0050] At 502, a high sputter yield material is optionally attached to the sample manipulator. In particular, a high sputter yield material such as copper may be attached to the sample manipulator in a chamber of a charged particle system, outside such a chamber, or a combination thereof. For example, the high sputter yield material may be attached to a probe portion of the sample manipulator using a gas deposition attachment where a precursor gas is introduced into a region between the sample manipulator and the high sputter yield material, and then a charged particle beam is used to deposit the precursor gas to form an attachment joint. In another exemplary process, the sample manipulator may be moved into close proximity to the high sputter yield material, a charged particle beam may be used to mill away a portion of the high sputter yield material adjacent to the sample, and the milled material may be deposited to form one or more attachment joints between the sample manipulator and the high sputter yield material.

[0051] Alternatively, in some embodiments of this process, rather than requiring step 502 to be performed, the sample manipulator is equipped with a probe constructed from a high sputter yield material (e.g., purchased with such a coating, or purchased without, if the coating is added by in situ or ex situ deposition).

[0052] At 504, the sample is brought into proximity with the sample manipulator. Specifically, the sample and / or the sample manipulator may be moved such that the portions of the sample manipulator that will be attached to the sample (e.g., the probe, the intermediate body made of the high sputter yield 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 may be attached to a moving component and / or otherwise configured to be translated, angled, and / or rotated.

[0053] At 506, the high sputter yield material is irradiated with a charged particle beam. Specifically, the charged particle beam is used to mill away one or more portions of the high sputter yield material while leaving one or more other portions of the high sputter yield material located close to the sample manipulator unmilled. In this manner, some portions of the high sputter yield material near the sample are removed while still leaving portions of the material within 10 microns, within 1 micron, or closer to the sample. For example, three portions located at the edge / surface of the high sputter yield material may be milled while two portions of the material located between the three portions may be left unmilled.

[0054] At 508, the milled high sputter yield material is redeposited to form an attachment joint between the sample and the sample manipulator. While and immediately after the portion of the high sputter yield material is milled away at step 506, the sample is held in a fixed position to allow the milled away material to settle on the high sputter yield material and / or the non-milled portion of the sample. In this manner, the milled material forms a deposit that interconnects to form an attachment joint between the high sputter yield material and the sample. By redepositing the milled material, one or more attachment joints may be created between the sample and the non-milled portion of the high sputter yield material that holds the sample in place. Not only are these attachment joints easy for the user to create / easily automated because they are created without the introduction of precursor gases or liquids, but this process 500 may be used to attach samples made of highly reactive materials to a support structure. Moreover, the process 500 allows the mounting joint to be performed at cryogenic temperatures and / or in a vacuum without the need for special microscope mechanisms to be developed or included in the charged particle system and without the user having to master complex processes.

[0055] At 510, the sample is optionally translated by a sample manipulator. For example, the sample manipulator may translate, angle, and / or rotate the sample so that the sample is in a desired position within the charged particle system.

[0056] 6A-C show different exemplary embodiments for creating an attachment between a sample manipulator and a sample in a charged particle system. For example, FIG. 6A depicts an example 610 in which a sample 612 is attached to a sample manipulator 614 that corresponds to a sample probe made of a high sputter yield material. In this manner, when a portion 616 of the sample probe proximate to 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.

[0057] FIG. 6B illustrates an embodiment 640 in which a sample 642 is attached to a sample manipulator corresponding to a sample probe 644 coated with a high sputter yield material 646. In this manner, when a portion 648 of the coating adjacent to the sample 642 is milled away, the milled material at least partially redeposits to form an attachment structure 650 between the sample 642 and the sample manipulator. FIG. 6C illustrates an embodiment 660 in which a sample 662 is attached to a sample manipulator corresponding to a sample probe 664 attached to an intermediate body 666 constructed from a high sputter yield material. When a portion 668 of the intermediate body 666 adjacent to the sample 642 is milled away, at least a portion of the milled material redeposits to form an attachment structure 670 between the sample 662 and the intermediate body 666.

[0058] FIG. 7 shows a series of images 700 illustrating an exemplary implementation of an exemplary process for sample lift-out and protective cap placement of highly reactive materials using a sample holder with a beveled edge. Image 702 shows an example of a sample holder 720 with a beveled edge 722. In accordance with 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 that a nested cavity 724 is prepared in the support structure 720 adjacent to the beveled edge 722. For example, the charged particle beam can be used to mill away material from the support structure 720 to create a hole, pocket, or inset volume into which a portion of the sample can be inserted.

[0059] Image 706 shows a sample 726 in the process of being translated with a sample manipulator 728 such that at least a portion of the sample 726 is positioned within the nested cavity 724. Specifically, image 706 shows an embodiment in which the sample 726 is attached to the sample manipulator 728 using an intermediate 730 made of a high sputter yield material, as shown and described in connection with Figures 5 and 6C. Image 708 shows the condition after the sample 726 has been translated such that at least a portion is positioned within the nested cavity 724, and the sample 726 is then attached to the sample holder 720 by milling away portions of the sample holder 732 adjacent to the sample such that the milled material is redeposited to form an attachment structure between the sample 726 and the sample holder 720.

[0060] Image 710 shows a cross-section of the situation depicted in image 708. Image 710 shows a cross-section of sample 726 and a thin portion of sample holder 734 extending along the surface of sample 726. Image 712 shows the use of a charged particle beam 736 to mill away a portion of sample 726 and a thin portion of sample holder 734 along a plane 738 to expose a surface of interest 740. In this manner, the thin portion of sample holder 734 acts as a protective cap through which the charged particle beam 736 initially impinges, thus reducing the curtaining effect on the region of interest 740. In some embodiments, the region of interest 740 may then be optionally imaged or otherwise investigated using an electron beam 742.

[0061] Examples of inventive subject matter according to the present disclosure are described in the paragraphs listed below.

[0062] A1. A method for performing sample lift-out and protective cap placement of a highly reactive material in a charged particle microscope system comprising preparing a nested cavity in a support structure, translating at least a portion of the sample into the nested cavity, and milling material from an area of ​​the support structure defining the nested cavity, whereby at least a portion of the material milled from the support structure is redeposited to form an attachment bond between the sample and a remainder of the support structure.

[0063] A2. The method of paragraph A1, wherein preparing the nested cavity includes milling away a volume of the support structure, the volume capable of receiving at least a portion of the sample.

[0064] A2.1. The method of paragraph A2, wherein the nested void is a hole and translating 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.

[0065] A2.2. The method of any one of paragraphs A2-A2.1, wherein the nested cavity is configured such that when an attachment bond is formed between the sample and the support structure, at least a portion of the sample is positioned where the volume of the sample that was milled away was located.

[0066] A2.3. The method of any one of paragraphs A2-A2.2, wherein a volume of the support structure is milled away with a focused ion beam.

[0067] A3. The method of any one of paragraphs A1-A2.3, further comprising performing one or more of serial sectioning tomography on the sample, enhanced insertable backscatter detector (CBS) analysis on the sample, chemical analysis, SIMS analysis, E-beam (EDX) analysis, Raman analysis, and electron backscatter diffraction (EBSD) analysis.

[0068] A3.1. The method of paragraph A3, wherein the method includes milling away a portion of the sample to expose a surface of interest; and imaging at least a portion of the surface of interest.

[0069] A3.1.1. The method of paragraph A3.1, wherein the milling is performed with a focused ion beam.

[0070] A3.1.2. The method of any one of paragraphs A3.1 through A3.1.1, wherein at least a portion of the support structure is used as a protective cap during milling of the sample.

[0071] A3.1.2.1. The method of paragraph A3.1.2, wherein using a portion of the support structure as a protective cap includes milling 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.

[0072] A3.1.2.1.1. The method of paragraph A3.1.2.1, wherein a portion of the sample is milled away using a high current mill with a FIB or plasma FIB.

[0073] A3.1.2.2. The method of any one of paragraphs A3.1.2 through A3.1.2.1.1, wherein using a 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.

[0074] A3.1.3. The method of any one of paragraphs A3.1-A3.1.2.2, wherein imaging includes irradiating at least a portion of the surface of interest with an electron beam.

[0075] A3.1.4. The method of any one of paragraphs A3.1 through A3.1.3, wherein the process further includes milling away an additional portion of the sample to expose an additional surface of interest.

[0076] A3.1.5. The method of any one of paragraphs A3.1 through A3.1.4, wherein the process further includes milling away multiple additional portions of the sample to expose multiple additional surfaces of interest.

[0077] A3.1.6. The method of any one of paragraphs A3.1 through A3.1.5, wherein milling away the portion of the sample is carried out at least in part using a rocking mill.

[0078] A4. The method of any one of paragraphs A1 through A3.1.6, wherein the support structure is a sample grid.

[0079] A4.1. The method of paragraph A4, wherein the sample grid is a TEM specimen grid.

[0080] A5. The method of any one of paragraphs A1 through A3.1.6, wherein the support structure is a sample holder.

[0081] A6. The method of any one of paragraphs A1 through A3.1.6, wherein the support structure is constructed at least in part from silicon.

[0082] A7. The method of any one of paragraphs A1 through A3.1.6, wherein the support structure is an aluminum block.

[0083] A8. The method of any one of paragraphs A1 through A3.1.6, wherein the support structure is constructed from an inert material that is not reactive to the focused ion beam.

[0084] A9. The method of any one of paragraphs A1-A3.1.6, wherein the support structure is a beveled holder having a beveled edge.

[0085] A9.1. The method of paragraph A9, wherein at least a portion of the beveled holder extends beyond the sample when the sample is inserted into the nested gap.

[0086] A9.2. The method of any one of paragraphs A9-A9.1, further including: milling away a section of the sample includes milling through the bevel edge using the bevel edge as a protective cap.

[0087] A9.3. Any one of the methods of paragraphs A9 through A9.2, where the bevel edge is milled at a 45 degree angle.

[0088] A9.4. The method of any one of paragraphs A9-A9.3, wherein the bevel edge can be created or the bevel edge can be commercially purchased.

[0089] A10. The method of any one of paragraphs A1-A9.4, wherein the sample is attached to the sample probe via an attachment coupling, and translating at least a portion of the sample into the nested gap includes translating the sample probe such that at least a portion of the sample is translated into the nested gap.

[0090] A10.1. The method of paragraph A10, further comprising milling away the attachment bond such that the sample is detached from the sample probe.

[0091] A10.2. The method of paragraph A10, further comprising 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 detached from the sample.

[0092] A11. The method of any one of paragraphs A1-A10.2, further comprising preparing a sample from the specimen.

[0093] A11.1. The method of paragraph A11, wherein preparing the sample from the specimen includes milling away a portion of the sample surrounding the area of ​​interest, attaching a sample probe to the area of ​​interest, and milling away a portion of the sample such that the area of ​​interest is no longer attached to the sample.

[0094] A11.1.1. The method of paragraph A11.1, wherein preparing the sample from the sample further includes translating the sample probe such that the region of interest is away from the sample.

[0095] A11.1.2. The method of any one of paragraphs A11.1 to A11.1.1, wherein the region of interest corresponds to a sample.

[0096] A11.1.3. Attaching the sample probe to the region of interest is any one of the methods of paragraphs A11.1 through A11.1.2, including any one of the methods of paragraphs B1 through B14.2.2.2.2.1.

[0097] A12. The method of any one of paragraphs A1 to A11.1.3, wherein the specimen corresponds to a battery or a part of a battery.

[0098] The method of paragraph A12, where the specimen corresponds to a lithium battery, a lithium ion battery, a battery anode, a battery cathode, a battery separator, or a combination thereof.

[0099] A13. The method of any one of paragraphs A1-A12.1, wherein the material includes at least one of lithium, magnesium, lithium polymer, lithium manganese oxide, lithium cobalt oxide, and lithium sulfide.

[0100] A14. The method of any one of paragraphs A1-A13, wherein the milling is performed with one of a focused ion beam and an electron beam.

[0101] A14.1. The method of paragraph A14, wherein the ion beam is a plasma focused ion beam.

[0102] B1. A method for creating an attachment between a sample manipulator and a sample in a charged particle system, comprising: translating the sample manipulator so that it is proximate to the sample, where a portion of the sample manipulator proximate to the sample is composed of a high sputter yield material; and milling the high sputter yield material with a charged particle beam such that a portion of the high sputter yield material is removed from the sample manipulator, where at least a portion of the removed high sputter yield material is redeposited to form the attachment between the sample manipulator and the sample.

[0103] B1.1. The method of paragraph B1, wherein the high sputter yield material corresponds to a material that, when irradiated with a particular ion species and voltage, produces a greater number of atoms / ions than silicon or tungsten.

[0104] B1.1.1. The method of paragraph B1.1, wherein the high sputter yield material corresponds to an emission rate of greater than 5, 7, 8, or 10 atoms / ion when the material is irradiated with a 30 kV focused ion beam.

[0105] 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.

[0106] B1.2. The method of any one of paragraphs B1 through B1.1.1.1, wherein the high sputter yield material is copper or brass.

[0107] B2. The method of any one of paragraphs B1-B1.2, wherein translating the sample manipulator includes translating the sample manipulator such that the portion comprised of the high sputter yield material is within 10 microns.

[0108] B2.1. The method of paragraph B2, wherein translating the sample manipulator includes translating the sample manipulator such that the portion comprised of the high sputter yield material is within 1 micron.

[0109] B3. The method of any one of paragraphs B1-B2.1, wherein the sample manipulator comprises a probe constructed from a high sputter yield material.

[0110] B4. The method of any one of paragraphs B1-B2.1, wherein the sample manipulator comprises a probe that is coated with a high sputter yield material.

[0111] B4.1. The method of paragraph B4, wherein irradiating the high sputter yield material includes milling away a portion of the coating adjacent the sample.

[0112] B5. The method of any one of paragraphs B1-B2.1, wherein the sample manipulator includes an intermediate body attached to the probe, the intermediate body being constructed from a high sputter yield material.

[0113] B5.1. The method of paragraph B5, wherein the intermediate is attached to a probe portion of the sample manipulator.

[0114] B5.1.1. The method of paragraph B5.1, wherein the intermediate is attached to the probe portion of the sample manipulator by gas deposition.

[0115] B5.1.2. Intermediates are

[0116] translating the probe portion such that the probe portion is adjacent to the intermediate portion;

[0117] The method of paragraph B5.1, wherein the intermediate is attached to a probe portion of the sample manipulator by a process including milling a portion of the intermediate adjacent to the probe with a charged particle beam, wherein at least a portion of the removed intermediate is redeposited to form an attachment between the probe portion and the intermediate.

[0118] B6. The method of any one of paragraphs B1-B5.1.2, wherein the charged particle beam is a focused ion beam.

[0119] B6.1. The method of paragraph B6, wherein the charged particle beam is a plasma focused ion beam.

[0120] B7. The method of any one of paragraphs B1 through B5.1.2, wherein the charged particle beam is an electron beam.

[0121] B8. The method of any one of paragraphs B1-B7, wherein the method for creating an attachment between a sample manipulator and a sample in a charged particle system requires a reduced amount of precursor gas than previous attachment methods.

[0122] B9. The method of any one of paragraphs B1-B8, wherein the attachment between the sample manipulator and the sample is formed without adding additional precursor gas to the system.

[0123] B10. The method of any of paragraphs B8 or B9, wherein the precursor gas includes platinum.

[0124] B11. The method of any one of paragraphs B1-B10, wherein the method is performed in a charged particle system at cryogenic temperatures.

[0125] B12. The method of any one of paragraphs B1-B11, wherein the method is performed in a charged particle system in a vacuum.

[0126] B13. The method of any one of paragraphs B1-B12, wherein the sample is a thin layer.

[0127] B14. The method of any one of paragraphs B1-B13, wherein milling the high sputter yield material includes milling a plurality of locations on the high sputter yield material proximate to the sample.

[0128] B14.1. The method of paragraph B14, wherein each of the plurality of locations is located at an edge of the high sputter yield material proximate the sample.

[0129] B14.2. The method of any one of paragraphs B14-B14.1, wherein there is at least one region of high sputter yield material along an edge proximate to the sample that is not milled away between the plurality of locations.

[0130] B14.2.1. The method of paragraph B14.2, wherein at least a portion of the removed high sputter yield material is redeposited to form an attachment between the specimen and at least one area of ​​high sputter yield material along an edge adjacent to the sample that is not milled away.

[0131] B14.2.2. The method of any one of paragraphs B14.2 through B14.2.1, wherein there are multiple regions of high sputter yield material along the edge of the sample adjacent to the sample that have not been milled away.

[0132] B14.2.2.1. The method of paragraph B14.2.2, wherein at least a portion of the removed high sputter yield material is redeposited to form an attachment between the specimen and more than one of the regions of high sputter yield material along an edge adjacent to the sample that is not milled away.

[0133] B14.2.2.2. The method of any one of paragraphs B14.2.2 through B14.2.2.1, wherein at least a portion of the removed high sputter yield material is redeposited to form a plurality of attachments between the sample and the high sputter yield material.

[0134] The method of paragraph B14.2.2.2, wherein each of the plurality of mountings connects the sample to a corresponding one of at least one region of high sputter yield material along an edge proximate to the sample that has not been milled away.

[0135] B14.2.2.2.2. A plurality of at least one area of ​​high sputter yield material along an edge adjacent to the sample that is not milled away, the method of any one of paragraphs B14.2.2.2 through B14.2.2.2.1.

[0136] The method of paragraph B14.2.2.2.2.1. wherein at least four attachments are formed between the sample and corresponding areas of high sputter yield material along the edge adjacent to the sample that are not milled away.

[0137] C1. A charged particle 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 irradiation by the charged particles; one or more processors; and memory storing non-transitory computer readable instructions that, when executed by the one or more processors, cause the one or more processors to perform any one of the methods of paragraphs A1-A14.1 and / or B1-B14.2.2.2.2.1.

[0138] C2. The charged particle system of paragraph C1, further comprising a vacuum chamber for housing the sample.

[0139] C2.1. The charged particle system of paragraph C2, wherein the instructions cause the one or more processors to perform the method of any of paragraphs A1 through A14.1 and / or B1 through B14.2.2.2.2.1 while the sample is in a vacuum.

[0140] C2.2. The charged particle system of paragraph C2, wherein the instructions cause the one or more processors to perform the method of any one of paragraphs A1 through A14.1 and / or B1 through B14.2.2.2.2.1 without breaking vacuum in the vacuum chamber.

[0141] C3. The charged particle system of any one of paragraphs C1-C2.2, wherein the instructions cause one or more processors to perform the method of any one of paragraphs A1-A14.1 and / or B1-B14.2.2.2.2.1 while the sample is at cryogenic temperatures.

[0142] D1. Use of the system of any one of paragraphs C1 to C3 to implement the method of any one of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

[0143] E1. A non-transitory computer-readable medium storing instructions that, when executed by a processor, cause the processor to begin performing the method of any one of paragraphs A1-A14.1 and / or B1-B14.2.2.2.2.1.

[0144] F1. Use of the non-transitory computer-readable medium of paragraph E1 to implement the method of any one of paragraphs A1 through A12.7 and / or B1 through B14.2.2.2.2.1.

Claims

1. 1. A method for performing sample lift-out and protective cap placement in a charged particle microscope system, comprising: preparing nested voids in a support structure, the preparation comprising milling away volumes of the support structure; translating at least a portion of the sample into the nested gap; and milling material from a region of the support structure that defines the nested void such that at least a portion of the material milled from the support structure redeposits to form an attachment bond between the sample and a remainder of the support structure.

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

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

4. The method comprises: milling away a portion of the sample to expose a surface of interest; The method of claim 1 , further comprising 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 cap during the milling of the sample.

6. 6. The method of claim 5, wherein using the portion of the support structure as a protective cap comprises 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 a 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 constructed from an inert material that is chemically inert to the focused ion beam.

9. The method of claim 1 , wherein the support structure is a beveled holder having a bevel edge, and the nested gap is prepared adjacent to the bevel edge.

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

11. 10. The method of claim 9, further comprising using the beveled edge as a protective cap by first milling away a section of the sample by milling through the beveled holder.

12. the sample is attached to a sample probe via a mounting coupling; 2. The method of claim 1, wherein translating the at least a portion of the sample into the nested gap comprises translating the sample probe such that the at least a portion of the sample is translated into the nested gap.

13. Attaching the sample probe to the sample includes: translating the sample probe so that the sample probe is proximate to the sample, a portion of the sample probe proximate to the sample being composed of a high sputter yield material; 13. The method of claim 12, comprising milling the high sputter yield material with a charged particle beam such that a portion of the high sputter yield material is removed from a sample probe, and at least a portion of the removed high sputter yield material is redeposited to form an attachment between the sample probe and the sample.

14. The sample probe comprises: a probe constructed from the high sputter yield material; a probe coated with the high sputter yield material; and an intermediate body attached to the probe.

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

16. 1. A charged particle system comprising: a charged particle emitter configured to emit charged particles toward the sample; a sample holder configured to support the sample; an optical column configured to direct the charged particles incident on the sample; a detector system configured to detect emissions from the sample due to irradiation 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: preparing nested voids in a support structure, the conditioning step comprising milling away volumes of the support structure; translating at least a portion of the sample into the nested gap; milling material from a region of the support structure, the region defining the nested void such that at least a portion of the material milled from the support structure redeposits to form an attachment bond between the sample and a remainder of the support structure.

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

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

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 cryogenic temperatures.

20. A non-transitory computer-readable medium storing instructions that, when executed by a processor, cause the processor to: preparing nested voids in a support structure, the conditioning step comprising milling away volumes of the support structure; translating at least a portion of the sample into the nested gap; and milling material from a region of the support structure that defines the nested void such that at least a portion of the material milled from the support structure is redeposited to form an attachment bond between the sample and a remainder of the support structure.

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