System and method for sample lift-out of highly reactive material

Abstract

To provide a method and system for performing sample lift-out and protective cap arrangement of highly reactive materials in a charged particle microscope system.SOLUTION: The method includes preparing a nested gap in a support structure, translating at least a portion of a sample into the nested gap, and milling material from an area of the support structure defining the nested gap. The material from the area of the support structure is milled such that at least a portion of the removed material is redeposited to form an attachment joint between the sample and the remaining part of the support structure. In various embodiments, the sample may be then investigated using one or more of continuous sectioning tomography on the sample, extended insertable backscatter detector (CBS) analysis on the sample, and electron backscatter diffraction (EBSD) analysis on the sample.SELECTED DRAWING: Figure 1

Description

Background Art

[0001] In scanning electron microscopes and transmission electron microscopes, a charged particle beam is used to image or otherwise investigate a region of interest on a sample. Often, before imaging and / or investigating the region of interest, it is necessary to prepare and / or manipulate the sample within the system to enable the region of interest to be exposed or otherwise prepared. In current systems, such preparation often involves one or more of preparing the sample from a larger specimen using the charged particle beam, attaching the sample to a manipulation probe to enable the sample to be translated 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 investigated.

[0002] In current systems, the sample is attached to the probe and / or sample holder using a precursor gas or a stored liquid. Specifically, in some attachment methods, a precursor gas is introduced into the volume surrounding the sample, where gas molecules form deposits on the sample, probe, and / or sample holder when irradiated with the charged particle beam. In another current attachment method, a liquid is first introduced onto the sample, probe, and / or sample holder, and the liquid is irradiated with the 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 have drawbacks that render them unsuitable for some microscopy investigations.

[0003] For example, a charged particle microscope system investigates a sample within a sealed chamber with respect to reducing contamination of optical components, reducing the effects of unwanted particles on the charged particle beam, and having unwanted deposits on the sample. The introduction of precursor gas and / or liquid adds additional material to the chamber of the charged particle microscope system, increasing these unwanted effects. In addition, introducing gas or liquid requires a specially adapted mechanism that complicates the design and implementation aspects of the new charged particle system, while also adding complex processing procedures that are difficult for new users to implement accurately. Finally, in the case of highly reactive samples, previous precursor gases cannot be used, as the introduction of gas can cause degradation of the sample surface and / or make the sample more reactive to the charged particle beam when subsequent milling or imaging is performed after attachment. For this reason, there is a need for new attachment and sample manipulation systems and processes that enable imaging and investigation of highly reactive materials.

SUMMARY OF THE INVENTION

[0004] A method and system for performing sample lift-out and protective cap placement of a highly reactive material within a charged particle microscope system are disclosed herein. The method includes preparing a nested void within a support structure, translating at least a portion of the sample into the nested void, and milling material from a region of the support structure that defines the nested void. 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 can then be investigated using one or more of serial sectioning tomography on the sample, extended insertable backscattered 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 a highly reactive material within a charged particle system may include 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 impinge on the sample, and a detector system configured to detect radiation from the sample due to irradiation by the charged particles. The system may further include 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, translate at least a portion of the sample into the nested void, and mill material from a region of the support structure that defines the nested void. BRIEF DESCRIPTION OF THE DRAWINGS

[0006] The detailed description is set forth with reference to the accompanying drawings. In the drawings, the leftmost digit of a reference number identifies the figure in which the reference number first appears. The same reference number in different figures indicates similar or identical items.

[0007]

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[0008] Like reference numerals refer to corresponding parts throughout several views of the drawings.

DETAILED DESCRIPTION OF THE INVENTION

[0009] A method and system for performing sample lift-out and protective cap placement of highly reactive materials within a charged particle microscope system are disclosed. More specifically, the present disclosure includes a method and system in which a nested void is created within a support structure, the sample is translated such that at least a portion of the sample is positioned within the nested void, and then material from a region of the support structure that defines the nested void is milled away. The material from the region of the support structure is positioned proximate the sample such that at least a portion of the removed material is redeposited to form one or more attachment joints between the sample and the remaining portion of the support structure. In this way, the sample can be attached to a sample holder without the need to add a precursor gas or other type of attachment medium to the charged particle system. Additionally, since the attachment is formed by passive redeposition of the milled material, the potential for reaction and / or other types of damage to the sample is much smaller. This enables a sample composed of a highly reactive material, such as 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 manner, one or more methodologies, such as, but not limited to, serial sectioning tomography on the sample, extended insertable backscattered detector (CBS) analysis on the sample, and electron backscattered diffraction (EBSD) analysis on the sample, can be used to image and / or investigate one or more regions of interest of the sample.

[0010] In addition, methods and systems for creating an attachment between a sample manipulator and a sample within a charged particle system are also disclosed herein. Specifically, the present disclosure includes methods and systems for attaching a sample to a holder or manipulator by irradiating a high sputter yield material proximate to the sample. First, the sample manipulator is translated such that a portion of the manipulator made of the high sputter yield material is positioned proximate to the sample (e.g., within microns). Next, the region 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, the high sputter yield material corresponds to a material that produces more atoms / ions than silicon or tungsten when irradiated with a particular ion beam species and voltage. For example, the high sputter yield material is defined as a material such as copper or zinc that emits more than 5, 7, 8, or 10 atoms / ions 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 illustrated with solid lines, whereas elements that are optional in a given example are illustrated with dashed lines. However, elements illustrated with solid lines are not necessarily essential to all examples of the present disclosure, and elements shown with solid lines may be omitted from a particular example without departing from the scope of the present disclosure.

[0012] FIG. 1 illustrates an exemplary system 100 for performing sample lift-out and protective cap placement of a highly reactive material 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 that includes 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 cap placement of a highly reactive material in situ. It should be noted that the present disclosure is not limited to an environment that includes a microscope, and in some embodiments, environment 100 may include different types of systems configured to manipulate and / or otherwise examine sample 108.

[0013] The exemplary microscope system 104 can be, or can include, one or more 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. FIG. 1 shows the exemplary microscope system 104 as a dual beam microscope system that includes a STEM column 110 and an FIB column 112.

[0014] FIG. 1 depicts an 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 source, a Schottky emission source, a field emission source, etc.) that emits an electron beam 114 toward the sample 108 along an electron emission axis 118. The electron emission axis 118 is a central axis that extends from the electron source 116 through the sample 108 along the length of the exemplary microscope system 104. FIG. 1 depicts the exemplary microscope system 104 as including the electron source 116, but in other embodiments, the STEM column 110 may comprise a charged particle source, such as an ion source, configured to emit a plurality of charged particles toward the sample 108.

[0015] Acceleration lens 120 accelerates / decelerates, focuses, and / or directs electron beam 114 toward electron beam focusing column 122. Electron beam focusing column 122 focuses electron beam 114 so that the electron beam is incident on at least a portion of sample 108. Additionally, focusing column 122 may correct and / or adjust aberrations (e.g., geometric aberrations, chromatic aberrations) of electron beam 114. In some embodiments, electron beam focusing column 122 may include one or more of an aperture, deflector, transmission lens, scanning coil, condenser lens, objective lens, etc. that simultaneously focus electrons from electron source 116 onto a small spot on sample 108. By adjusting the direction of the electron beam by the deflector and / or scanning coil, various locations of sample 108 can be scanned. In this way, electron beam 114 can function as an imaging beam that is scanned across the surface layer of the sample (i.e., the surface of the layer that is close to STEM column 104 and / or irradiated by electron beam 114). This irradiation of the surface layer of sample 108 causes the component electrons of electron beam 114 to interact with the component electrons / molecules / features of the sample, whereby the component electrons / molecules / features cause sample 108 to emit emissions 124. The particular emissions that are emitted are based on the corresponding elements / molecules / features that cause them, whereby the emissions can be analyzed to determine information regarding the corresponding elements / molecules. Additionally, although FIG. 1 illustrates emissions 124 as moving downstream of sample 108, one of ordinary skill in the art will understand that the emissions can be emitted in other directions, including, but not limited to, toward charged particle source 116.

[0016] FIG. 1 further illustrates detector systems 126(a) and 126(b) for detecting emissions 124 resulting from an electron beam 114 incident on a 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 can be configured to detect different types of emissions, or different parameters of the emissions can 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] FIG. 1 also depicts an exemplary microscope system 104 as including an FIB column 112 for removing portions of a sample 108 or other object in a microscope chamber 130. For example, the FIB column 112 may mill away portions of the sample body to expose or otherwise create the sample 108. In other embodiments, the exemplary microscope system 104 may include other types of delayer components, such as lasers, mechanical blades (e.g., diamond blades), electron beams, and the like. The FIB column 112 is shown as including a charged particle emitter 132 configured to emit a plurality of ions 134 along an ion emission axis 136.

[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 having one or more of an aperture, a deflector, a transmission lens, a scanning coil, a condenser lens, an objective lens, etc., which focus the ions from the charged particle emitter 132 onto a small spot on the sample 108 all at once. In this way, the elements in the ion focusing column 138 can cause one or more portions of the sample 108 or other body to be milled away or otherwise removed from the ions emitted by the charged particle emitter 132. For example, the FIB column 112 can be configured to remove the surface layer of the sample 108 having a known thickness from the sample 108 during image acquisition during slice and view imaging.

[0019] FIG. 1 illustrates an 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 the 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 the sample or specimen is attached and / or otherwise held. Additionally, the sample manipulator 108 is a mechanism 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 shows the sample manipulator as having a probe portion extending from the body and to which the sample can be attached. The sample loading chamber 142 can be sealable from the microscope chamber 130 and the sample holder 140 can be retracted into the sample loading chamber 142 such that the user can access and / or interact with the sample holder 140 while the sample holder 140 is in the sample loading chamber 142.

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

[0021] One or more of the computing devices 128 can be components of the exemplary microscope system 104, can be devices separate from the exemplary microscope system 104 that communicate with the exemplary microscope system 104 via a network communication interface, or can be a combination thereof. For example, the exemplary microscope system 104 can include a first computing device 128 that is a component part of the exemplary microscope system 104 and that functions as a controller to drive the operation of the exemplary charged particle microscope system 104 (e.g., adjusting the scanning location on the sample by operating the scanning coil). In such an embodiment, the exemplary microscope system 104 can also include a second computing device 128 that is a desktop computer separate from the exemplary microscope system 104 and that is executable to process data received from the detector system 126 to generate an image of the sample 108 and / or to perform other types of analysis or post-processing of the detector data. The computing device 128 can be further configured to receive user selections via a keyboard, mouse, touchpad, touch screen, and the like. The computing device 128 is configured to generate an image of the surface layer of the sample 108 within the exemplary microscope system 104 based on data and / or data signals from the detector system 126.

[0022] In addition, computing device 128 is configured to control FIB column 112, sample manipulator 106, and / or sample holder 140 to enable the implementation of sample lift-out and protective cap placement for highly reactive materials within charged particle microscope system 104. For example, computing device 128 may cause FIB column 112 to mill nested voids into a support structure (e.g., a sample grid, sample holder, or other structure that enables imaging / investigating a sample when the sample is attached) using a plurality of ions 134. Based on one or more user selections, automation programs, or combinations thereof, computing device 128 can translate (e.g., translate, angle, and / or rotate) sample holder 140 or sample manipulation device 106 such that at least a portion of sample 108 is positioned within the nested void. When sample 108 is positioned at least partially within the nested void, computing device 128 may cause FIB column 112 to mill away portions of the support structure that are near a portion of the sample and / or that define the nested shape. A user selection, automation program, or combination thereof selects the portion of the support structure such that as a result of being milled in this way, the milled material redeposits into the nested void to form an attachment bond between the support structure and the portion of sample 108. In this way, an interconnection is formed between sample 108 and the support structure, such that sample 108 is held in place for further processing / imaging without the need to add deposition gas or other materials to microscope chamber 130. In some embodiments, computing device 128 may be further configured to cause exemplary microscope system 104 to prepare sample 108 prior to attachment (e.g., remove the sample from a larger sample body and expose the surface / structure of interest), process the sample to prepare it for imaging / investigation, or perform imaging / investigation of one or more regions of sample 108.

[0023] Alternatively, or in addition, computing device 128 may be configured to create one or more attachment portions between sample manipulator 106 and sample 108 within charged particle system 104 without the need to add additional deposition gas or other materials to microscope chamber 130. For example, computing device 128 may cause a high sputter yield material (e.g., copper) to be positioned proximate to sample 108. The high sputter yield material may optionally be attached to the sample manipulator, which itself may comprise the high sputter yield material (e.g., purchased with such a coating or, if the coating is added by in situ or ex situ deposition, purchased without).

[0024] A user selection, automation program, or combination thereof may then cause computing device 128 to activate FIB column 112 to mill away portions of the high sputter yield material proximate to the sample while leaving one or more other portions of the high sputter yield material positioned proximate to the sample manipulator un-milled. In this way, some portions of the high sputter yield material near the sample are removed while material portions still remain within 10 microns, within 1 micron, or closer to the sample. Thus, when the milled high sputter yield material re-deposits, 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. One of ordinary skill in the art will understand that the computing architecture 150 may be implemented on a single computing device 128 or may span multiple computing devices. For example, the individual modules and / or data configurations depicted in the computing architecture 150 may be executed by and / or stored on various computing devices 128. In this way, the various process steps of the methods of the invention disclosed herein may be executed and / or implemented by separate computing devices 128 and in various orders within the scope of this disclosure. In other words, the functions realized by the illustrated components can, in some implementations, be combined into fewer components or distributed among additional components. Similarly, in some implementations, the functions of some of the illustrated components may not be realized and / or other additional functions may be made available.

[0026] In an exemplary computing architecture 150, a computing device includes one or more processors 152 and a memory 154 communicatively coupled to the one or more processors 152. Although not intended to be limiting, the exemplary computing architecture 150 is shown as including a control module 156 stored in the memory 154. As used herein, the term "module" is intended to represent an exemplary subdivision of executable instructions for purposes of discussion and is not intended to represent any type of requirement or required methodology, manner, or arrangement. Thus, although various "modules" are described, their functions and / or similar functions can be arranged differently (e.g., combined into fewer modules, divided into more modules, etc.). Further, although specific functions and modules are described herein as being implemented by software and / or firmware executable on a processor, in other instances, any or all of the modules can be implemented in whole or in part by hardware (e.g., special 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 can be executed across a plurality of 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 to carry out system functions or maintenance. In some embodiments, the control module 156 may cause the exemplary microscope system 204 to perform sample lift-out and / or protective cap placement of highly reactive materials 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 annotations regarding 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 gas 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 annotations regarding FIGS. 5-7.

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

[0029] Memory 154 accessible to one or more processors 152 is an example of a computer-readable medium. A computer-readable medium can include two types of computer-readable media, namely 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 the storage of information such as computer-executable instructions, data structures, program modules, or other data. Computer storage media can include, but is not limited to, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EEPROM), flash memory or other memory technologies, compact disc read-only memory (CD-ROM), digital versatile disc (DVD), or other optical storage, magnetic cassettes, magnetic tape, magnetic disk storage devices or other magnetic storage devices, or any other non-transmission medium that can be used to store desired information and can be accessed by a computing device. Generally, computer storage media can include computer-executable instructions that, when executed by one or more processing units, cause the 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] One of ordinary skill in the art will also recognize that an item or portion of an item may be transferred between the memory 154 and other storage devices for purposes of memory management and data integrity. Alternatively, in other implementations, some or all of the software components may execute in memory on another device and communicate with the computing device 128. Some or all of the system components or data structures may also be stored on a non-transitory computer-accessible medium or on a portable product readable by a suitable drive (e.g., as instructions or structured data), examples of which are described above. In some embodiments, instructions stored on a computer-accessible medium separate from the computing device 128 may be transmitted to the computing device 128 via a transmission medium or signal such as an electrical, electromagnetic, or digital signal carried via a communication medium such as a wireless link. Various implementations may further include receiving, transmitting, or storing instructions and / or data that implement according to the previous description of computer-accessible media.

[0031] FIGS. 2 and 5 are flow diagrams of illustrative processes shown as collections of blocks of a logical flow graph representing a series of operations that may be implemented in hardware, software, or a combination thereof. In a software context, a block represents 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 the process.

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

[0033] In 202, the sample is optionally prepared. For example, the sample may be pre-treated to expose a region of interest that is to be imaged and / or investigated. In some embodiments, this may include forming the sample using a process such as a sample lift-out procedure that mills away a portion of the sample from a larger sample to expose a chunk that includes the region of interest, where the chunk is attached to a sample manipulator, the chunk is separated from the body of the sample, and the sample manipulator and / or the sample are translated such that the chunk moves away from the sample body. Alternatively, or in addition, the surface of the sample may be milled and / or polished to expose the region of interest and / or remove damage from the surface to enable high-quality imaging / investigation. 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] In 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 capable of accommodating 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 fitting volume into which a portion of the sample can be inserted. In some embodiments, the support structure can be a sample holder having a bevel edge (e.g., a 45-degree bevel edge), and the nested void can be a portion of the sample holder near the bevel edge milled away by a focused ion beam. Such a nested void can be milled such that at least a portion of the beveled holder extends beyond the sample when the sample is inserted into the nested void.

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

[0036] In 206, the sample is translated such that at least a portion of the sample is positioned within the nested void. For example, the sample can be attached to a movable sample manipulator (e.g., a sample probe) that is translated, angled, and / or rotated such that at least a portion of the sample is received within the nested void. That is, the sample is positioned such that the portion of the sample is located within the volume where the milled-away portion of the support structure was located.

[0037] At 208, a portion of the support structure is milled away. Specifically, a portion of the support structure that is near a portion of the sample and / or that defines a nested void is milled away from the support structure. In some embodiments, the edge / surface of the support structure that defines the nested void is 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 projections of the support structure remain proximate to the sample between the milled portions.

[0038] At 210, the milled material is redeposited to form an attachment joint between the sample and the support structure. While and immediately after a portion of the support structure is milled away at step 208, the sample is held in a fixed position such that the milled material is deposited onto the support structure and / or non-milled portions of the sample. In this way, the milled material can form a deposit that interconnects to form an attachment joint between the support structure and the sample. In this way, by redepositing the milled material, one or more attachment joints can be created between the sample and the non-milled portion of the support structure that holds the sample in place. Since these attachment joints are created without the introduction of a precursor gas or liquid, these attachment joints are not only easy for the user to create / easily automated, but also the sample composed of highly reactive materials can be attached to the support structure using this process 200.

[0039] At 212, the sample is optionally processed to prepare the sample for imaging and / or investigation. For example, a portion of the sample can be milled away with a charged particle beam to expose a region 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 has been imaged / investigated, the sample can be further processed one or more additional times such 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 the charged particle beam first mills through a portion of the support structure before beginning to remove a portion of the sample. In this way, the portion of the support structure can be used as a protective cap to prevent curtaining of the exposed sample surface. Thus, in addition to creating attachment joints without introducing precursor gas, process 200 can also enable utilization of the protective cap without introducing precursor gas. In some embodiments, processing the sample can 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 can include milling away a portion of the sample probe such that the tip of the sample probe remains attached to the sample and the remaining portion of the sample probe is detached from the sample.

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

[0041] Figures 3 and 7 are visual flow diagrams illustrating exemplary processes for performing sample lift-out and protective cap placement of highly reactive materials according to the present disclosure. Specifically, FIG. 3 shows a series of captured images 300 that illustrate an exemplary implementation of the exemplary process 200 described in the annotations regarding FIG. 2.

[0042] Image 302 shows an optional creation of a sample 320 from a sample body 322. Specifically, image 302 shows a state in which one or more volumes 324 of the sample body 322 surrounding the sample 320 have been milled away using a charged particle beam (e.g., an ion beam). Image 304 shows a subsequent state of an exemplary process in which a sample manipulator 326 is attached to the sample 320. For example, the sample 320 can be attached to the sample manipulator 326 using a deposition gas or by an attachment process described in connection with FIG. 5. When the sample 320 is attached to the sample manipulator 326, the final portion 328 of the sample, which was connected to the sample body, is milled away. In this way, when the sample 320 is completely separated from the sample body, the sample manipulator 326 can translate the sample 320 away from the sample body 322.

[0043] Image 306 shows a state in which a nested void 330 is prepared in the support structure 332. For example, a charged particle beam can be used to mill away material from the support structure 332. The nested void 330 can correspond to a hole, pocket, cavity, or fitting volume into which a portion of the sample can be inserted. Although not shown in Image 306, in some embodiments, the nested void can correspond to a region adjacent to and / or abutting a raised structure / portion of the support structure, such that when the sample is translated into the nested void, a portion of the sample is proximate to and / or abuts the raised structure / portion of the support structure. In various embodiments, the support structure 332 can correspond to one or more of a sample grid, a sample holder, or other structure that enables imaging / investigating the sample when the sample is attached. The support structure can be at least partially composed of many different materials including, but not limited to, silicon, aluminum, copper, etc.

[0044] Image 308 shows a state after the sample 320 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 void 330. The sample is shown as being 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 void 330.

[0045] Image 310 shows the state of Image 308 with a plurality of milling locations 334 mapped onto Image 308. Specifically, Image 310 shows a plurality of milling locations 334 each corresponding to a portion of the support structure 332 that is to be milled using a charged particle beam. Image 312 shows the state of the process after the portion 334 of the sample holder 332 has been milled away, and the milled material is redeposited to form an attachment joint 336 between the sample 320 and the support structure 332.

[0046] Figures 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 prior art. Figure 4A is an image 410 of sample 320 from Figure 3, after the sample 320 has been further processed and prepared for imaging and / or investigation of the sample 320. For example, a portion of the sample 320 was milled away with a charged particle beam to expose a clean surface 412 of the region of interest of the sample, and then polished to remove damage from the surface of the sample. Specifically, Figure 4A shows an embodiment in which a portion of the sample 320 is 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 where the sample is composed of both stable and reactive materials, first, milling through the stable material can be performed, whereby the stable material functions as a cap that reduces curtaining at the clean reactive surface 412(a). Alternatively, in some embodiments, milling can be performed such that a portion of the support structure 322 is first penetrated and milled, whereby the support structure 322 functions as a cap that reduces curtaining at the clean reactive surface 412(a). Using the processes described herein, high - quality EBSD maps and / or band contrast maps that were not previously possible with conventional techniques can be obtained for the clean surface 412 of highly reactive materials.

[0047] In addition, in some embodiments the processes described herein have been shown to maintain the crystallinity of highly reactive materials, as evidenced by the obtained Kikuchi patterns of portions of such clean surfaces 408. Figure 4B shows an image 420 in which a sample 422 is inserted into a nested void 424 in a support structure 426 and attached using the techniques according to the present disclosure. Figure 4B further shows the use of 428 to assist in user processing and / or automated processing and investigation of the region of interest in the sample 422.

[0048] Figure 4C shows the results of sample lift-out and protective cap placement of a highly reactive material using prior art techniques. As can be seen, when an 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 of the prior art system. First, the sample 434 can be damaged by reaction with external materials (e.g., deposition gas, binding liquid) introduced to form the attachment. Second, even if the damage caused by the introduction of such external materials is not catastrophic, upon irradiation with a charged particle beam, the reaction between the external material and the highly reactive material 434 can cause the surface of the sample 434 to undergo a subsequent catastrophic reaction. As shown in image 430, due to these reactions, prior art techniques for in-situ attachment of samples are not effective for highly reactive materials.

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

[0050] At 502, optionally, attach a high sputter yield material to the sample manipulator. Specifically, a high sputter yield material such as copper can be attached to the sample manipulator within the chamber of the charged particle system, outside such a chamber, or a combination thereof. For example, when a precursor gas is introduced into the region between the sample manipulator and the high sputter yield material, the high sputter yield material can be attached to the probe portion of the sample manipulator using a gas deposition attachment portion, and then the precursor gas is deposited using a charged particle beam to form an attachment joint. In another exemplary process, the sample manipulator can be moved to be extremely close to the high sputter yield material, and a portion of the high sputter yield material proximate to the sample can be milled away using a charged particle beam, and the milled material can be fixed to form one or more attachment joints between the sample manipulator and the high sputter yield material.

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

[0052] At 504, bring the sample close to the sample manipulator. Specifically, the sample and / or the sample manipulator can be moved such that a portion of the sample manipulator (e.g., a probe, an intermediate made of the high sputter yield material attached in step 502, etc.) that will be attached to the sample 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 a moving component and / or configured otherwise to be translated, angled, and / or rotated.

[0053] At 506, irradiate the high sputter yield material with a charged particle beam. Specifically, while using the charged particle beam to mill away one or more portions of the high sputter yield material, leave one or more other portions of the high sputter yield material located adjacent to the sample manipulator unmilled. In this way, some portions of the high sputter yield material near the sample are removed, while material portions still remain 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 can be milled, while two portions of the material located between the three portions can be left unmilled.

[0054] At 508, redeposit the milled high sputter yield material to form an attachment joint between the sample and the sample manipulator. While portions of the high sputter yield material are being milled away in step 506 and immediately thereafter, the sample is held in a fixed position so as to deposit the milled away material onto the high sputter yield material and / or the non-milled portions of the sample. In this way, deposits are formed on the milled material, and the deposits interconnect to form an attachment joint between the high sputter yield material and the sample. By redepositing the milled material, one or more attachment joints can be created between the sample and the non-milled portions of the high sputter yield material that hold the sample in a predetermined position. Since these attachment joints are created without the introduction of a precursor gas or liquid, these attachment joints are not only easy for the user to create / easily automated, but also the sample made of a highly reactive material can be attached to a support structure using this process 500. Moreover, this process 500 enables the implementation of attachment joints at cryogenic temperatures and / or in a vacuum without the need to develop or include a special microscope mechanism in the charged particle system and without the user having to acquire a complex process.

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

[0056] Figures 6A - C show different exemplary embodiments for creating an attachment between a sample manipulator and a sample within a charged particle system. For example, Figure 6A depicts an embodiment 610 where a sample 612 is attached to a sample manipulator 614 corresponding to a sample probe made of a high sputter yield material. In this way, when a portion 616 of the sample probe adjacent to the sample 612 is milled away, the milled material at least partially redeposits to form an attachment structure 618 between the sample 612 and the sample manipulator 614.

[0057] Figure 6B depicts an embodiment 640 where 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 way, 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. Figure 6C depicts an embodiment 660 where a sample 662 is attached to a sample manipulator corresponding to a sample probe 664 attached to an intermediate 666 composed of a high sputter yield material. When a portion 668 of the intermediate 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 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 a highly reactive material using a sample holder having a bevel edge. Image 702 shows an embodiment of a sample holder 720 having a bevel edge 722. According to the present invention, the bevel edge can be at any angle less than 90 degrees. In some embodiments, a charged particle beam can be used to mill away a portion of the sample holder 720 to create the bevel edge 722. Image 704 shows a state in which a nested void 724 is prepared in a support structure 720 proximate the bevel 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 fitting volume into which a portion of the sample can be inserted is created.

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

[0060] Image 710 shows a cross-section of the state 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 a state in which a portion of sample 726 and the thin portion of sample holder 734 are milled away along plane 738 using charged particle beam 736 to expose surface of interest 740. In this way, the thin portion of sample holder 734 functions as a protective cap through which charged particle beam 736 first passes and thus can reduce the catenation effect on region of interest 740. In some embodiments, region of interest 740 can then optionally be imaged using electron beam 742 or otherwise investigated.

[0061] Examples of the subject matter of the invention according to this 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 within a charged particle microscope system, the method comprising preparing a nested void in a support structure, translating at least a portion of the sample into the nested void, and milling material from a region of the support structure that defines the nested void, whereby at least a portion of the material milled from the support structure is redeposited to form an attachment joint between the sample and the remaining portion of the support structure.

[0063] A2. Preparing the nested void includes milling away a volume of the support structure, the volume being capable of receiving at least a portion of the sample, the method of paragraph A1.

[0064] A2.1. 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, the method of paragraph A2.

[0065] The nested voids are configured such that when an attachment joint is formed between the sample and the support structure, at least a portion of the sample is positioned where the volume of the milled-away sample was located, according to any one of the methods of paragraphs A2 to A2.1.

[0066] A volume of the support structure is milled away using a focused ion beam, according to any one of the methods of paragraphs A2 to A2.2.

[0067] The method further includes performing one or more of a serial sectioning tomography method on the sample, an extended insertable backscattered detector (CBS) analysis on the sample, a chemical analysis, a SIMS analysis, an electron beam (EDX) analysis, a Raman analysis, and an electron backscatter diffraction (EBSD) analysis, according to any one of the methods of paragraphs A1 to A2.3.

[0068] 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, according to the method of paragraph A3.

[0069] The milling is performed using a focused ion beam, according to the method of paragraph A3.1.

[0070] At least a portion of the support structure is used as a protective cap during the milling of the sample, according to any one of the methods of paragraphs A3.1 to A3.1.1.

[0071] Using a portion of the support structure as a protective cap includes positioning the focused ion beam such that a portion of the support structure is milled before a portion of the sample is milled away by the focused ion beam, according to the method of paragraph A3.1.2.

[0072] A portion of the sample is milled away using a high-current mill with FIB or plasma FIB, according to the method of paragraph A3.1.2.1.

[0073] Using a part of the support structure as a protective cap is one of the methods in paragraphs A3.1.2 to A3.1.2.1.1 that prevents the tail of the focused ion beam from milling away a part of the sample.

[0074] Imaging involves irradiating at least a part of the surface of interest with an electron beam, and is the method described in any one of paragraphs A3.1 to A3.1.2.2.

[0075] The process further includes milling away an additional part of the sample to expose an additional surface of interest, and is the method described in any one of paragraphs A3.1 to A3.1.3.

[0076] The process further includes milling away a plurality of additional parts of the sample to expose a plurality of additional surfaces of interest, and is the method described in any one of paragraphs A3.1 to A3.1.4.

[0077] Milling away a part of the sample is carried out at least partially using a rocking mill, and is the method described in any one of paragraphs A3.1 to A3.1.5.

[0078] The support structure is a sample grid, and is the method described in any one of paragraphs A1 to A3.1.6.

[0079] The sample grid is a TEM sample grid, and is the method described in paragraph A4.

[0080] The support structure is a sample holder, and is the method described in any one of paragraphs A1 to A3.1.6.

[0081] The support structure is at least partially composed of silicon, and is the method described in any one of paragraphs A1 to A3.1.6.

[0082] A7. The support structure is an aluminum block, in any one of the methods of paragraphs A1 to A3.1.6.

[0083] A8. The support structure is composed of an inert material that does not react to a focused ion beam, in any one of the methods of paragraphs A1 to A3.1.6.

[0084] A9. The support structure is a beveled holder having a bevel edge, in any one of the methods of paragraphs A1 to A3.1.6.

[0085] A9.1. When the sample is inserted into the nested void, at least a portion of the beveled holder extends beyond the sample, in the method of paragraph A9.

[0086] A9.2. Milling away a section of the sample further includes milling through the bevel edge using the bevel edge as a protective cap, in any one of the methods of paragraphs A9 to A9.1.

[0087] A9.3. The bevel edge is milled at an angle of 45 degrees, in any one of the methods of paragraphs A9 to A9.2.

[0088] A9.4. The bevel edge can be created or the bevel edge can be a commercially available product, in any one of the methods of paragraphs A9 to A9.3.

[0089] A10. The sample is attached to the sample probe via an attachment joint, and translating at least a portion of the sample into the nested void includes translating the sample probe so that at least a portion of the sample is translated into the nested void, in any one of the methods of paragraphs A1 to A9.4.

[0090] A10.1. The method of paragraph A10 further includes milling away the attachment joint so that the sample is detached from the sample probe.

[0091] 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 remaining portion of the sample probe is separated from the sample.

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

[0093] The method of paragraph A11, wherein preparing a sample from the specimen includes the steps of milling away a portion of the specimen surrounding the region of interest, attaching a sample probe to the region of interest, and milling away a portion of the specimen such that the region of interest becomes detached from the specimen.

[0094] The method of paragraph A11.1, wherein preparing a sample from the specimen further includes translating the sample probe so that the region of interest moves away from the specimen.

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

[0096] The method of any one of paragraphs A11.1 - A11.1.2, wherein attaching the sample probe to the region of interest includes any method of paragraphs B1 - B14.2.2.2.2.1.

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

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

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

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

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

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

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

[0104] The method of paragraph B1.1, wherein the high sputter yield material corresponds to a sputter rate 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 the focused ion beams of Ga+, Xe+, Ar, N+, Cs+, Bi+, or O+.

[0106] B1.2. The method of any one of paragraphs B1 to B1.1.1.1 where the high sputtering yield material is copper or brass.

[0107] B2. Translating the sample manipulator includes translating the sample manipulator so that the part composed of the high sputtering yield material is within 10 microns, according to any one of paragraphs B1 to B1.2.

[0108] B2.1. Translating the sample manipulator includes translating the sample manipulator so that the part composed of the high sputtering yield material is within 1 micron, according to the method of paragraph B2.

[0109] B3. The sample manipulator comprises a probe made of a high sputtering yield material, according to any one of paragraphs B1 to B2.1.

[0110] B4. The sample manipulator comprises a probe coated with a high sputtering yield material, according to any one of paragraphs B1 to B2.1.

[0111] B4.1. Irradiating with a high sputtering yield material includes milling and removing the part of the coating close to the sample, according to the method of paragraph B4.

[0112] B5. The sample manipulator comprises an intermediate body attached to the probe, and the intermediate body is made of a high sputtering yield material, according to any one of paragraphs B1 to B2.1.

[0113] B5.1. The intermediate body is attached to the probe part of the sample manipulator, according to the method of paragraph B5.

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

[0115] B5.1.2. The intermediate body is

[0116] translating the probe part so that the probe part approaches the intermediate body,

[0117] milling a part of the intermediate body close to the probe with a charged particle beam, wherein at least a part of the removed intermediate body is redeposited to form an attachment between the probe part and the intermediate body, and the method of paragraph B5.1, which is attached to the probe part of the sample manipulator, including milling.

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

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

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

[0121] B8. 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 previous attachment methods, and is any one of the methods of paragraphs B1 to B7.

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

[0123] B10. The method according to either B8 or B9, wherein the precursor gas contains platinum.

[0124] B11. The method according to any one of paragraphs B1 to B10, wherein the method is carried out in a charged particle system at extremely low temperatures.

[0125] B12. The method according to any one of paragraphs B1 to B11, wherein the method is carried out in a charged particle system under vacuum.

[0126] B13. The sample is a thin layer, by any one of the methods of paragraphs B1 to B12.

[0127] B14. Milling a high sputter yield material includes milling a plurality of locations on the high sputter yield material adjacent to the sample, by any one of the methods of paragraphs B1 to B13.

[0128] B14.1. Each of the plurality of locations is located at an edge of the high sputter yield material adjacent to the sample, by the method of paragraph B14.

[0129] B14.2. There is at least one region of the high sputter yield material along an edge adjacent to the sample that has not been milled away between the plurality of locations, by any one of the methods of paragraphs B14 to B14.1.

[0130] B14.2.1. At least a portion of the removed high sputter yield material is redeposited to form an attachment portion between the sample and at least one region of the high sputter yield material along an edge adjacent to the sample that has not been milled away, by the method of paragraph B14.2.

[0131] B14.2.2. There are a plurality of regions of the high sputter yield material along an edge of the sample adjacent to the sample that have not been milled away, by any one of the methods of paragraphs B14.2 to B14.2.1.

[0132] B14.2.2.1. At least a portion of the removed high sputter yield material is redeposited to form an attachment portion between the sample and a plurality of at least one region of the high sputter yield material along an edge adjacent to the sample that has not been milled away, by the method of paragraph B14.2.2.

[0133] In one of the methods of paragraphs B14.2.2 to B14.2.2.1, at least a portion of the removed high sputter yield material is redeposited to form a plurality of attachment portions between the sample and the high sputter yield material.

[0134] In the method of paragraph B14.2.2.2, each of the plurality of attachment portions connects the sample to a corresponding one of at least one region of the high sputter yield material along an edge of the sample that has not been removed by milling and is close to the sample.

[0135] In one of the methods of paragraphs B14.2.2.2 to B14.2.2.2.1, a plurality of regions of the high sputter yield material along an edge of the sample that has not been removed by milling and is close to the sample.

[0136] In the method of paragraph B14.2.2.2.2, at least four attachment portions are formed between the sample and a corresponding region of the high sputter yield material along an edge of the sample that has not been removed by milling and is close to the sample.

[0137] A charged particle system comprising: a charged particle emitter configured to emit charged particles towards a sample; a sample holder configured to support the sample; an optical column configured to direct the charged particles to be incident on the sample; a detector system configured to detect emissions from the sample due to irradiation by the charged particles; one or more processors; and a memory storing non-transitory computer-readable instructions which, when executed by the one or more processors, cause the one or more processors to perform one of the methods of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

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

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

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

[0141] The command C3 causes one or more processors to perform, while the sample is at cryogenic temperature, any one of the methods of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1 in any one of the charged particle systems of paragraphs C1 to C2.2.

[0142] Use of any one of the systems of paragraphs C1 to C3 for performing any one of the methods of paragraphs A1 to A14.1 and / or B1 to B14.2.2.2.2.1.

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

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

[0145] [Appendix 1] A method for performing sample lift - out and protective cap placement within a charged particle microscope system, preparing a nested void in a support structure, translating at least a portion of the sample into the nested void, Milling a material from the 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 is redeposited to form an attachment joint between the sample and the remaining portion of the support structure, the method comprising milling. [Appendix 2] Preparing the nested void includes milling away a volume of the support structure that can receive at least a portion of the sample, 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 volume, the method according to Appendix 1. [Appendix 3] The nested void is configured such that when the attachment joint is formed between the sample and the support structure, at least a portion of the sample is positioned at the location where the volume of the milled sample was located, the method according to Appendix 2. [Appendix 4] The method further includes: Milling away a portion of the sample to expose a surface of interest; Imaging at least a portion of the surface of interest, the method according to any one of Appendices 1 to 3. [Appendix 5] At least a portion of the support structure is used as a protective cap during the milling of the sample, the method according to Appendix 4. [Appendix 6] Using the portion of the support structure as a protective cap includes positioning the focused ion beam such that the portion of the support structure is milled before the portion of the sample is milled away by the focused ion beam, the method according to Appendix 5. [Appendix 7] The support structure is one of a sample grid, a sample holder, and an aluminum block, the method according to any one of Appendices 1 to 6. [Appendix 8] The method according to Appendix 7, wherein the support structure is composed of an inert material that does not chemically react with the focused ion beam. [Appendix 9] The method according to any one of Appendices 1 to 8, wherein the support structure is a bevelled holder having a bevel edge, and the nested void is prepared in proximity to the bevel edge. [Appendix 10] The method according to Appendix 9, wherein when the sample is inserted into the nested void, at least a portion of the bevelled holder extends beyond the sample. [Appendix 11] The method according to Appendix 9, further comprising using the bevel edge as a protective cap by milling away a section of the sample by first milling through the bevelled holder. [Appendix 12] The method according to any one of Appendices 1 to 11, wherein the sample is attached to a sample probe via an attachment joint, and translating at least a portion of the sample into the nested void includes translating the sample probe such that at least a portion of the sample is translated into the nested void. [Appendix 13] Attaching the sample probe to the sample includes a step of translating the sample probe so that the sample probe is in proximity to the sample, wherein a portion of the sample probe in proximity to the sample is composed of a high sputter yield material; and a step of milling the high sputter yield material with a charged particle beam so that a portion of the high sputter yield material is removed from the sample manipulator, and at least a portion of the removed high sputter yield material is redeposited to form an attachment portion between the sample probe and the sample. The method according to Appendix 12. [Appendix 14] The sample probe is a probe composed of the high sputter yield material, a probe coated with the high sputter yield material, an intermediate attached to the probe, and includes one of them, the method according to Appendix 13. [Appendix 15] The sample is the method according to any one of Appendices 1 to 14, corresponding to a battery, battery raw material, or a part of a battery. [Appendix 16] A charged particle system, a charged particle emitter configured to emit charged particles towards a sample, a sample holder configured to support the sample, and an optical column configured to guide the charged particles to be incident on the sample, a detector system configured to detect the emission from the sample due to irradiation by the charged particles, one or more processors, a memory storing non - transient computer - readable instructions, and includes, When the non - transient computer - readable instructions are executed by the one or more processors, the one or more processors are caused to perform the step of preparing an nested void in a support structure, perform the step of translating at least a part of the sample into the nested void, perform the step of milling a material from a region of the support structure, the region defining the nested void such that at least a part of the material milled from the support structure is redeposited to form an attachment joint between the sample and the remaining part of the support structure. A charged particle system. [Appendix 17] The nested void is configured such that at least a portion of the sample is positioned at a location where the volume of the milled-away sample was located when the attachment joint is formed between the sample and the support structure, the charged particle system according to appended claim 16. [Appended claim 18] The charged particle system according to appended claim 16, further comprising a vacuum chamber for housing the sample, wherein the instruction causes the one or more processors to perform the step while the sample is in a vacuum state. [Appended claim 19] The charged particle system according to appended claim 16, wherein the instruction causes the one or more processors to perform the step while the sample is at cryogenic temperature. [Appended claim 20] A non-transitory computer-readable medium storing instructions which, when executed by a processor, cause the processor to prepare a nested void in a support structure; translate at least a portion of a sample into the nested void; mill a material from a region of the support structure, the region defining the nested void such that at least a portion of the milled material from the support structure is redeposited to form an attachment joint between the sample and the remaining portion of the support structure, and initiate performance of the milling step, the non-transitory computer-readable medium.

Claims

1. A method of creating an attachment between a sample manipulator and a sample within a charged particle system, comprising: translating the sample manipulator so that the sample manipulator is proximate to the sample, wherein a portion of the sample manipulator proximate to the sample is composed of a high sputter yield material; milling the high sputter yield material with a charged particle beam to remove a portion of the high sputter yield material from the sample manipulator, wherein at least a portion of the removed high sputter yield material is redeposited to form an attachment between the sample manipulator and the sample without milling material from the sample; A method comprising the above steps.

2. The method according to claim 1, wherein the high sputter yield material corresponds to a material that produces a greater number of atoms / ions than silicon or tungsten when irradiated with a specific ion species and voltage. The method according to claim 1.

3. The method according to claim 2, wherein the high sputter yield material corresponds to an emission rate of greater than 5, 7, 8, or 10 atoms / ions when the material is irradiated with a 30 kV focused ion beam. The method according to claim 2.

4. The method according to claim 3, wherein the 30 kV focused ion beam is one of a focused ion beam of Ga+, Xe+, Ar, N+, Cs+, Bi+, or O+. The method according to claim 3.

5. The step of translating the sample manipulator includes translating the sample manipulator such that the portion composed of the high sputter yield material is within 10 microns. The method according to claim 1.

6. The sample manipulator comprises a first probe composed of the high sputter yield material, or The sample manipulator comprises a second probe coated with the high sputter yield material that defines a coating, and irradiating the high sputter yield material includes milling away a portion of the coating proximate to the sample. The method according to claim 1.

7. The sample manipulator comprises an intermediate attached to a probe, the intermediate being composed of the high sputter yield material. The method according to claim 1.

8. The intermediate is attached to a probe portion of the sample manipulator. The intermediate is attached to the probe portion of the sample manipulator by gas deposition or The intermediate is attached to the probe portion of the sample manipulator translating the probe portion so that the probe portion is close to the intermediate; milling, with the charged particle beam, a portion of the intermediate proximate to the probe, wherein at least a portion of the removed intermediate is redeposited to form an attachment between the probe portion and the intermediate, the milling step; is attached by a process comprising The method according to claim 7.

9. The charged particle beam is a focused ion beam including a plasma focused ion beam, or an electron beam, The method according to claim 1.

10. The sample includes a lamella, the attachment between the sample manipulator and the sample is formed without adding an additional precursor gas containing platinum to the charged particle system; the method is performed in the charged particle system at cryogenic temperatures, or the method is performed in the charged particle system in a vacuum; The method according to claim 1.

11. The step of milling the high sputter yield material includes milling a plurality of locations on the high sputter yield material proximate to the sample, each of the plurality of locations is located at an edge of the high sputter yield material proximate to the sample, The method according to claim 1.

12. there is at least one region of the high sputter yield material along the edge proximate to the sample that has not been milled away between the plurality of locations, The method according to claim 11.

13. at least a portion of the removed high sputter yield material is redeposited to form an attachment between the sample and at least one region of the high sputter yield material along the edge proximate to the sample that has not been milled away, there are a plurality of regions of the high sputter yield material along the edge of the sample proximate to the sample that have not been milled away, The method according to claim 12.

14. A non-transitory computer-readable medium storing instructions, wherein when the instructions are executed by a processor, the processor is caused to: Translate the sample manipulator so that the sample manipulator is close to the sample, and a portion of the sample manipulator close to the sample is made of a high sputter yield material; Use a charged particle beam to mill the high sputter yield material, removing a portion of the high sputter yield material from the sample manipulator, and at least a portion of the removed high sputter yield material is redeposited to form an attachment portion between the sample manipulator and the sample without milling and removing material from the sample; A non-transitory computer-readable medium for causing an operation to be performed. [

15. ] At least a portion of the removed high sputter yield material is redeposited to form a plurality of attachment portions between the sample manipulator and the sample. The non-transitory computer-readable medium according to claim 14. [

16. ] The plurality of attachment portions connect the sample to at least a portion of the high sputter yield material along an edge of the sample that is not milled away and is close to the sample. The non-transitory computer-readable medium according to claim 15. [

17. ] A charged particle system, A charged particle emitter configured to emit a charged particle beam toward a sample; A sample holder configured to support the sample; An optical column configured to direct 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; A memory storing non-transitory computer-readable instructions, The instructions, when executed by the one or more processors, cause the one or more processors to: Translate the sample manipulator so that the sample manipulator is close to the sample, and a portion of the sample manipulator close to the sample is made of a high sputter yield material; Use the charged particle beam to mill the high sputter yield material, removing a portion of the high sputter yield material from the sample manipulator, and at least a portion of the removed high sputter yield material is redeposited to form an attachment portion between the sample manipulator and the sample without milling and removing material from the sample; Perform an operation, the memory, A charged particle system comprising...

18. Further comprising at least one region of the high sputter yield material along an edge adjacent to the sample that has not been milled away, At least four attachment portions are formed between the sample and at least one region of the high sputter yield material, The charged particle system according to claim 17.

19. There are a plurality of regions of the high sputter yield material along the edge adjacent to the sample that have not been milled away, The charged particle system according to claim 18.

20. At least a part of the removed high sputter yield material is redeposited to form a plurality of attachment portions between the sample and the high sputter yield material, The charged particle system according to claim 17.

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