Non-air transfer of solid state batteries and electrical testing of solid state batteries in scanning electron microscopes

Abstract

The disclosure relates to air transfer free of solid state batteries and electrical testing of solid state batteries in scanning electron microscopes. In one embodiment, an apparatus includes a sample stage including a base member and a sample support assembly coupled to the base member, where the sample support assembly includes a bracket having opposing first and second bracket portions, the first holder portion and the second holder portion are configured to compress a sample within the holder receiving portion, wherein the base member is configured to engage a sample stage within a microscope chamber. A method includes securing a sample stage in a microscope chamber and charging and / or discharging the sample at least partially through an electrical coupling in the chamber.

Description

Technical Field

[0001] This area is the testing of samples in a controlled environment. Background Art

[0002] In many charged particle beam microscopy and processing applications, samples need to be processed in an environment separate from the vacuum-controlled chamber of the charged particle beam microscope, as well as transported cleanly between environments. Unfortunately, existing solutions often fail to maintain sample cleanliness or other required sample conditions, or they require laborious or inefficient steps to process or test the sample. These problems are particularly pronounced in battery and battery-related samples. Therefore, there remains a need for improved techniques and equipment that overcome these shortcomings. Summary of the Invention

[0003] According to one aspect of the disclosed technology, an apparatus includes a sample carrier comprising a base member and a sample support assembly coupled to the base member, wherein the sample support assembly includes a bracket having opposing first and second bracket portions, the first and second bracket portions configured to compress a sample within a bracket receiving portion, wherein the base member is configured to engage a sample stage within a microscope chamber.

[0004] According to another aspect of the disclosed technology, an apparatus includes a sample carrier receiver including a support member having a base member and a receiving portion, the base member being coupled to a stage within a microscope chamber, the receiving portion being coupled to the base member, wherein the receiving portion includes a sliding mount extending at an oblique angle relative to the base member to receive and secure the sample carrier relative to the sample stage within the microscope chamber through slidable engagement with the sliding mount, and wherein the receiving portion includes an electrical coupling portion coupled to an electrical coupling portion of the sample carrier to provide an electrically conductive path from the sample carrier through the stage.

[0005] According to another aspect of the disclosed technology, a method includes: coupling an airless transfer container to an airless transfer container transfer port of a microscope vacuum chamber, wherein the airless transfer container stores a sample carrier; inserting the sample carrier from the airless transfer container into the microscope vacuum chamber by moving the sample carrier into a sample carrier receiver mounted on a sample stage located in the vacuum chamber; and electrically connecting an electrical coupling portion on the sample carrier and an electrical coupling portion on the sample carrier receiver.

[0006] According to another aspect of the disclosed technology, a method includes: securing a sample carrier to a sample stage within a microscope chamber, wherein the sample carrier includes a sliding member and a sample support assembly connected to the sliding member, wherein the sample support assembly includes a bracket having a first bracket portion and a second bracket portion relative to each other, the first bracket portion and the second bracket portion being configured to compress the sample within a bracket receiving portion, wherein the securing includes: slidably engaging the sliding member to a sample carrier receiver connected to the sample stage, and electrically coupling the sample carrier and corresponding electrical coupling portions of the sample carrier receiver; and charging and / or discharging the sample at least partially via the electrical coupling.

[0007] The foregoing and other objects, features and advantages of the disclosed technology will become more apparent from the following detailed description made with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Figure 1 is a schematic diagram of an example charged particle beam microscope.

[0009] Figures 2A to 2C is a schematic side view of an example sample carrier and receiver system.

[0010] Figures 3A to 3B is a schematic side view of another example sample carrier and receiver system.

[0011] Figure 4 is a perspective view of a sample carrier coupled to a sample receiver.

[0012] Figure 5 is a perspective view of another sample carrier engaged to a sample receiver having an angled configuration.

[0013] Figure 6 is a flow chart of an example method for transferring a sample carrier from an airless transfer container into a vacuum chamber.

[0014] Figure 7 is a flow chart of an example method for processing and experimenting with battery samples. DETAILED DESCRIPTION

[0015] Representative examples use a vacuum-controlled shuttle transport system to allow electrical testing and compression of solid-state batteries inside a scanning electron microscope (SEM). As used herein, “vacuum controlled” generally refers to a system with the ability to control the vacuum level in an internal volume, including with respect to a selected substance (such as air, nitrogen, an inert gas, etc.). Small compression elements such as piezoelectric actuators are incorporated into a portion of the shuttle of the vacuum-controlled shuttle transport system. The compression element can then be used to compress samples of solid-state batteries or button cells that are being electrically tested (in some examples, including during simultaneous SEM imaging) in a vacuum-controlled chamber of the SEM. Various examples can be combined with air-free transfer of solid-state battery samples using a vacuum-controlled shuttle transport system, electrical testing in the SEM (e.g., charge and discharge cycles), control of the compression pressure acting on the electrodes of the solid-state battery sample (e.g., in MPa), and / or simultaneous SEM imaging. The example can effectively provide SEM imaging of battery structural changes with respect to changes in compression pressure and charge / discharge parameters.

[0016] Solid-state batteries (SSBs) are a promising emerging technology that can offer increased power density, reduced size, and reduced weight compared to current batteries that rely on liquid electrolytes for ion transport. An SSB includes a solid separator between an anode and a cathode that acts as a medium through which ions move. In addition, one or more of the anode or cathode may be formed from a solid continuous layer of a material such as lithium metal. During operation of the SSB, ion transport may result in the accumulation of additional solid material (e.g., lithium metal) on the anode. For example, the thickness of the anode may change by tens of microns during charging. One of the key challenges in the production of SSBs is to produce a battery structure that is sufficiently sealed to ensure good contact between the layers (e.g., anode, separator, and cathode) while also allowing the size of the anode layer to expand and contract during charging and discharging.

[0017] The systems and methods of the present disclosure enable the preparation and measurement of the layer morphology and composition of samples such as SSBs over a range of experimental conditions, which can include electrical state (i.e., charged, discharged, or transient between charged states), temperature, vacuum pressurization, and applied compressive pressure.

[0018] The examples taught herein can be used to provide direct insights into changes in solid-state batteries during charge and discharge. For example, the optimal operating conditions of an SSB can be strongly dependent on the pressure between the electrodes, which, in selected examples, can be controlled using, for example, a compression element. In some examples, the compression element can adjust the compression on the SSB in response to changes in internal pressure within the SSB as a result of anode expansion due to material accumulation during operation of the SSB. This adjustment can be based on experimental design to apply a desired pressure, or the same pressure can be maintained before and after anode expansion.

[0019] The examples taught herein may also enable samples (e.g., SSBs) to be safely prepared outside a charged particle microscope under continuous application of vacuum pressure and / or compressive pressure and subsequently inserted into the charged particle microscope for measurement or imaging. Solid-state batteries (SSBs) may include components that are highly reactive with ambient air and may present a fire or explosion hazard if exposed to air. For example, the anode of an SSB may be formed from a solid layer of lithium metal. The example sample supports taught herein may apply compressive pressure to the sample while it is being cut or polished to expose the anode while the sample is outside the charged particle microscope. Such cutting or polishing may be performed under vacuum or inert gas conditions. The sample stage may then be inserted into the charged particle microscope under airless conditions while still applying compressive pressure to the sample.

[0020] The examples may be small and compact, allowing for precise placement of a battery sample into a holder that may already be located outside the microscope in an associated glove box used for manipulating and processing the battery sample.

[0021] In some conventional systems, a large compression stage is located in the SEM chamber. In some arrangements, insertion into a large stage already present in the chamber requires restoring the vacuum pressurization to atmospheric levels in order to place the sample in the chamber. This process results in a significant delay while the chamber is evacuated and then pumped back to vacuum conditions. In addition, the sample is not compressed during the time it is inserted and positioned in the stage located in the chamber. The loss of compression applied to the sample (i.e., during the time the sample is placed in the large compression stage) can adversely affect the experimental results. For example, if the compression between the electrode and the electrolyte (diaphragm) is lost, the original electrical properties of the SSB can be significantly altered. The systems and methods described herein overcome these problems by enabling the sample to be inserted into a charged particle microscope under air-free conditions while continuous compression is applied to the sample (i.e., without interrupting the application of compression).

[0022] In disclosed examples, the battery sample can be transferred without contact with air, for example, by placing the sample in a chamber of an SEM while the chamber is under vacuum. In many examples, the testing and imaging steps can be further combined with heating and / or cooling the sample in the chamber of the SEM. For example, some systems taught herein can include a heating and / or cooling element (e.g., a thermoelectric cooler or heater) that can adjust the temperature of the sample in the range of 30K to 450K.

[0023] Various examples can provide for maintained and / or adjustable compressive pressure applied to the sample during airless transport (e.g., from a glove box or BIB polisher to a SEM vacuum chamber). For SSB experiments (such as those conducted with pouch cells), such applied pressure can be beneficial. The pouch of a pouch cell typically does not ensure sufficient pressure is applied during battery cycling (even with intact pouch cells) so that compressive force applied during the charge cycle improves performance and may be necessary during experiments. Furthermore, compression may be more important where portions of the pouch are removed to allow SEM imaging of sample cross sections and related experiments. Furthermore, where a pouch is not provided for SSB according to some experiments (e.g., conducted with open cells), compression may be required for successful analysis. Furthermore, such compression can be provided during sample transfer to prevent delamination during transfer and during possible broad ion beam polishing prior to delivery to a SEM or other analytical tool.

[0024] In some examples, a sample holder mounted in a vacuum chamber of an SEM that receives a shuttle from a vacuum-controlled shuttle transport system is pre-tilted at an inclined angle (e.g., 45 degrees). This arrangement is particularly beneficial in a multi-beam SEM, such as a two-beam or three-beam focused ion beam (FIB) system that includes separate electrons, focused ion beams (such as plasma FIBs), and / or laser columns. The angled arrangement can allow a shuttle to be transferred with the sample holder angled to the internal moving stage so that, for example, a button cell or battery sample can be transferred in a flat position perpendicular to the z-axis of the electron beam column. The moving stage can then be returned to the flat position so that the sample is then angled relative to the z-axis of the electron beam column so that it is aligned perpendicularly to the beam axis of the PFIB and / or laser column. The shuttle can allow for airless transfer of button cells (e.g., CR2032) or similarly sized batteries between a glove box and a microscope chamber (e.g., the vacuum chamber portion of a FIB, SEM, or other charged particle microscope system) (e.g., under argon or vacuum), electrical contacting of battery samples inside the vacuum chamber of a microscope (e.g., for charging / discharging during testing), PFIB preparation of battery sample cross-sections in a rotary milling mode (provided by pre-tilting), and / or in combination with a low-temperature stage that can accelerate and improve PFIB processing characteristics. In some examples, PFIB milling can be performed in a cross-sectional direction (e.g., through the battery sample) and / or in a planar direction (e.g., surface milling).

[0025] Figure 11 is an example charged particle beam microscope 100 that includes three beam columns 102a, 104a, and 106a that can generate electron, ion, and photon beams 102b, 104b, and 106b, respectively, along corresponding beam axes 102c, 104c, and 106c. Axes 102c, 104c, and 106c are typically arranged at predetermined angles relative to one another, such as axes 104c and 106c shown, each arranged at 45 degrees relative to axis 102c, to direct corresponding beams 102b, 104b, and 106b into a sample region 108 within a pressure-controlled vacuum chamber 110. It should be understood that other angles are possible and need not be the same in the three-beam example. Other example angles may include 52 degrees, 30 degrees, 40 degrees, 60 degrees, 90 degrees, 110 degrees, and the like. In some examples, the angles may be adjustable, for example, using hinges. A sample stage, such as a translation stage 112, is located in the vacuum chamber 110 to control and manipulate the positioning of a sample 114 in the sample region 108, e.g., relative to the beams 102b, 104b, 106b. The sample 114 is mounted on a movable sample carrier 116 (which may also be referred to as a shuttle), which is coupled to a sample carrier receiver 118 that is mounted to or is part of the translation stage 112.

[0026] The sample carrier 116 with the mounted sample 114 can be transported into the vacuum chamber 110 using a vacuum-controlled shuttle transport system 120 (e.g., in the form of an airless transfer container). In many workflows, the sample 114 mounted on the sample carrier 116 can be processed in another location, such as a glove box 122, a wide ion beam polishing device, etc. After the transport system 120 is coupled to the vacuum chamber transport interface 124, the transport system 120 can be used to move the sample carrier 116 (e.g., via translation) into the vacuum chamber 110 to the sample area 108 to engage the sample carrier receiver 118 (e.g., via slidable contacts). In many examples, the sample carrier 116 can include conductive pathways 126 that couple components of the sample carrier 116 (such as one or more compression actuators) and / or the sample 114 (such as a sample electrode) to electrical interfaces 128, which can be aligned with and coupled to electrical interfaces 130 on the sample carrier receiver 118. The electrical interfaces 130 can be coupled to one or more power sources via, for example, conductive pathways 132 inside and / or outside the vacuum chamber 110. The conductive pathways 126, 132 can allow the sample 114 to be transported into the vacuum chamber 110 and electrically tested therein while maintaining a vacuum-controlled environment surrounding the sample 114 throughout the transport and testing process.

[0027] In some examples, the sample carrier receptacle 118 includes an angled extension that receives the sample carrier 116. During transport of the sample carrier 116 into the vacuum chamber 110, the moving stage 112 can rotate the sample carrier receptacle 118 to a rotational position such that the angled extension can receive the sample carrier 116 from the transport system 120, e.g., in a predetermined aligned position that allows for sliding engagement. The rotational position can provide the sample 114 in an imaging and / or processing position relative to (e.g., perpendicular to) the electron beam axis 102c. After the sample carrier 116 is coupled to the sample carrier receptacle 118, the moving stage 112 can rotate the sample carrier 116 (and the sample 114) to an alternative position, such as a flat position or a default position of the moving stage 112. With axes 104c, 106c at a common angle (e.g., 45 degrees) with axis 102c, translation stage 112 can produce a rotation about axis 102c to provide sample 114 in a processing position (e.g., perpendicular) relative to either beam 104b, 106b.

[0028] A control environment 134 may be coupled to or part of the microscope 100 and include a processor and memory 136 configured to control various components of the microscope 100, such as beam control 138, sample positioning using a motion stage 140, compression actuation 142, and sample powering (such as charging / discharging). In some examples, the compression actuation 142 may be controlled to provide a constant compressive pressure to the sample 114, such as during charging / discharging of the sample 114, where the sample 114 is a battery or button cell. In other examples, the applied compressive pressure may be controllably varied, for example, relative to the charge / discharge voltage, current, or other experimental parameters, based on pressure sensor feedback 144 from a pressure sensor that is part of the sample carrier 116 and coupled to the sample 114 to detect the applied compressive force. In some examples where the sample carrier receptacle 118 includes an angled extension, the angle of the extension may be controllably adjusted 146 by the control environment, for example, using an actuator coupled to a hinge that allows adjustment of the angle of the extension. In some examples, such hinges may also correspond to mechanically adjustable hinges.

[0029] Figures 2A to 2CAn example sample carrier and receiver system 200 is illustrated that can be used to test a sample 202, such as a button cell battery or a solid-state battery (SSB). System 200 can include a sample carrier 204 and an associated sample carrier receiver 206, which can be used in various examples herein. Sample carrier 204 can be used with a vacuum-controlled transport system that transports sample carrier 204 within and between vacuum-controlled environments. Sample carrier receiver 206 can be positioned in various environments, such as a vacuum chamber of a charged particle beam apparatus, a glove box, and a wide ion beam polisher, to receive sample carrier 204 from the vacuum-controlled transport system.

[0030] Specimen carrier 204 may include a base member 208 including a surface 210 that may be configured to slidably engage an associated receiving surface 212 of specimen carrier receiver 206. Specimen carrier 204 may be slid into a secure position, for example, by having a surface 214 that contacts a surface 216 of a stop 218. Stop 218 may have various forms (such as one or more abutments, detents, latches, snaps, detents, pin mechanisms, etc.) that prevent undesired movement of specimen carrier 204 during imaging and / or processing.

[0031] The sample carrier 204 may also include a first support portion 220 and a second support portion 222, as well as first and second electrical contacts 224 and 226, which may face and contact corresponding electrode surfaces 228a and 228b of the sample 202 disposed in a support receiving portion 229 of the sample carrier 204. A compression actuator 230 may be coupled to the first support portion 220 to compress the sample 202, for example, by forming a vise between the first and second support portions 220 and 222, as shown. For example, the first and second support portions may be attached to the base member 208 so as to provide expansion / contraction between the first support portion 220 and the electrical contacts 224. Movement of the electrical contacts 224 toward the sample 202, while constrained by the first and second support portions 220 and 222, results in compression of the sample 202. In some examples, the compression actuator 230 may also be coupled to the second support portion 222. In some examples, a pressure sensor 232 can be positioned relative to the compression actuator 230 (e.g., between the compression actuator 230 and the electrical contact 224) to detect the compressive pressure applied to the electrical contact 224 and thereby to the sample 202. Various compression actuators (such as piezoelectric actuators, linear motors, etc.) can be used, particularly where a sufficiently small form factor can be provided. In some examples, the compression actuator 230 provides an amount of compressive pressure in the range of 1 MPa to 10 MPa. In some examples, the compression actuator 230 can apply a force of approximately 1 kN. In some examples, the compression actuator 230 can have a travel range of at least 15 μm to compensate for material buildup on the anode of the SSB during charging.

[0032] Figures 2B to 2C Also shown are electrically conductive paths 234, 236, 238, 240 extending from first and second electrical contacts 224, 226, pressure sensor 232, and compression actuator 230, respectively, to electrical engagement portion 242. In some examples, electrical engagement portion 242 may be disposed at surface 214 such that, when sample carrier 204 is slidably engaged with sample carrier receiver 206 (see FIG. Figure 2C216 ), one or more contact surfaces of the electrical engagement portion 242 can be conductively coupled to one or more mating or corresponding contact surfaces of the electrical engagement portion 244 disposed at the surface 216 of the stopper 218. The electrical engagement portion 244 can be coupled to electrical conductive paths 246, 248, 250, 252, which are electrically connected to corresponding conductive paths 234, 236, 238, 240. The paths 234, 236, 238, 240, 246, 248, 250, 252 can be used to transmit power and / or electrical signals to / from various components of the sample carrier 204. In a representative example, the sample 202 can be a battery sample (e.g., an SSB, a button cell, etc.) that is charged and discharged using the compression actuator 230 to apply a compressive force on the sample 202 relative to the charge and discharge. In many examples, the compressive pressure applied to the sample 202 is maintained constant during charging / discharging (such as during an experiment in a microscope chamber), during transport, and / or during handling. In other examples, the compressive pressure applied to the sample can be controllably varied, for example, with respect to a charge / discharge cycle. Pressure sensor 232 can be used to provide feedback for monitoring and / or controlling the compressive pressure applied to sample 202. In some examples, the pressure is maintained at a constant pressure during expansion / contraction. In other examples, the pressure can be varied with respect to expansion / contraction.

[0033] Figures 3A to 3B Another example of a sample carrier and receiver system 300 that can be used to test a sample 302, such as a battery sample, is illustrated. System 300 can include many similar components to system 200, although different components can also be used. For example, system 300 can include a sample carrier 304 and an associated sample carrier receiver 306. Sample carrier 304 can include a base member 308. Sample carrier 304 can be slid into a secure position coupled to sample carrier receiver 306. Sample carrier 304 can include first and second support portions 310, 312 and first and second electrical contacts 314, 316 that can face and contact corresponding electrode surfaces 318a, 318b of sample 302 disposed in a support receiving portion 319 of sample carrier 304.

[0034] The first and second compression actuators 320 and 322 can be coupled to the first and second bracket portions 310 and 312, respectively, for example, by forming a vise between the first and second bracket portions 310 and 312. For example, the first and second bracket portions 310 and 312 can be attached to the base member 308 so as to provide expansion / contraction between the first bracket portion 310 and the electrical contacts 314, and to provide relative expansion / contraction between the second bracket portion 312 and the electrical contacts 316. Movement of the electrical contacts 314 and 316 toward the sample 202 results in compression of the sample 302 while being constrained by the first and second bracket portions 310 and 312. In some examples, a pressure sensor 324 and / or a pressure sensor 326 can be positioned relative to the compression actuators 320 and 322 to detect the compressive pressure applied to the electrical contacts 314 and 316, and thereby to the sample 302.

[0035] Figure 3B Electrically conductive paths 328, 330, 332, 334, 336, 338 are shown extending from the first and second electrical contacts 314, 316, the pressure sensors 324, 326, and the compression actuators 320, 322, respectively, to the electrical junction portion 340. The electrical junction portion 340 can be conductively coupled to an opposing electrical junction portion 342. The electrical junction portion 342 can be coupled to electrical conductive paths 344, 346, 348, 350, 352, 354, which are electrically connected to corresponding conductive paths 328, 330, 332, 334, 336, 338. The paths 328, 330, 332, 334, 336, 338, 344, 346, 348, 350, 352, 354 can be used to transmit power and / or signals to / from various components of the sampler carrier 304.

[0036] Figure 4 4 is another example of a sample carrier and receiver system 400. System 400 includes a sample carrier 402 and a sample carrier receiver 404. Sample carrier 402 can include a base member 406 that can be capable of slidingly engaging sample carrier receiver 404. Sample carrier 402 can slide in direction 405 to a secure position with a stop 408, which can include an edge 410 that fits within a corresponding slot 413 of sample carrier receiver 404. Sample carrier 402 includes first and second support portions 412, 414 and first and second electrical contacts 416, 418 that can face and contact an electrode surface of a sample (not shown) positioned between electrical contacts 416, 418 in a support receiving portion 419.

[0037] A compression actuator 420 can be coupled to the first bracket portion 412 to compress the sample by translating the first electrical contact 416 toward the second electrical contact 418. The second bracket portion 414 can be fixedly coupled to the base member 406. The first bracket portion 412 and the second bracket portion 414 can be coupled to translate relative to each other using linear sliding bearings (e.g., using an arrangement of one or more shafts 422a-422d that can be journaled about corresponding slotted portions of the first bracket portion 412 or the second bracket portion 414). The compression actuator 420 can be coupled to the base member 406 to provide stable translation of the first electrical contact 416.

[0038] With sample carrier 402 engaged with sample carrier receiver 404, first electrical contacts 416 and second electrical contacts 418 may be coupled to sample carrier receiver 404 via conductive pathways through sample carrier 402 (such as through base member 406). First electrical contacts 416 and second electrical contacts 418 may be conductively coupled 424, 426 to electrodes 428, 430 on sample carrier receiver 404 via stop 408 (with the pathway hidden) or another portion of sample carrier 402. For example, one or more pins 432a-432e may extend or be configured to extend to sample carrier receiver 404 at the engagement location, such as pins 432a, 432e extending to electrodes 428, 430.

[0039] Figure 5 is an example of a sample carrier and receiver system 500 that includes a sample carrier receiver 502 coupled to a sample stage, such as a translation stage 504, to receive a sample carrier 506. Sample carrier receiver 502 may include a base member 508 that may be coupled to translation stage 504 and an angled extension 510 that extends to provide a platform for receiving sample carrier 506 at a predetermined angle relative to base member 508. In some examples, the angle may be adjustable.

[0040] Base member 508 can be heated and / or cooled using an associated temperature control system coupled to (e.g., beneath or as part of) base member 508. Thus, in many such examples, the heating / cooling contacts can be independent of sample carrier 506 and the electrical contact pins associated with the sample carrier. In other examples, a resistive heater, Peltier cooling chip, or the like can be part of sample carrier 506, such that they share one or more pins or electrical contacts of sample carrier 506.

[0041] Figure 6is an example of a method 600 for transporting a transfer container (such as any of the sample carriers described herein). The example method may include various steps performed individually and in combination with other steps. At 602, an airless transfer container is engaged with an airless transfer container transfer port of a microscope vacuum chamber, and a sample carrier is contained in the airless transfer container in a vacuum-controlled environment. In other words, "airless" may generally refer to a vacuum-controlled environment, which may also be controlled under other conditions (such as nitrogen, argon, etc.). At 604, the sample carrier is inserted from the airless transfer container into the microscope vacuum chamber by moving the sample carrier into a sample carrier receptacle mounted on a sample stage located in the vacuum chamber (e.g., by being able to slidably engage the sample carrier receptacle). At 606, an electrical connector on the sample carrier is electrically coupled to an electrical connector on the sample carrier receptacle. In some examples, the various steps may be performed alternatively or additionally. For example, before or after the electrical connection at 606 (e.g., before or after an experiment in a microscope vacuum chamber), the sample can be processed at 608 in a vacuum and / or in the presence of an inert gas. The processing can be mechanical, chemical, or involve optical-based operations using a laser or ion beam. For example, the processing can be performed in a glove box, a wide ion beam polisher, or a preparation / processing chamber. In many examples, compressive pressure can be applied to the sample while the processing occurs or as part of the processing workflow. At 610, the sample mounted on the sample carrier can be transferred from the processing chamber to an airless transfer container under vacuum pressure and / or in the presence of an inert gas.

[0042] In a glove box (such as the one discussed at 608), a sample (such as a battery) can be mounted and compressed in a sample carrier. This can provide maintained contact between the electrodes of the sample and the electrolyte (particularly for SSBs), which can avoid negative effects on the performance of the sample being tested. For example, a pre-pressurized compression can be applied during installation (producing approximately 1 MPa in the battery, although other values ​​are possible, such as between 0.1 MPa and 5 MPa). In some examples, this pressure can be measured by a pressure sensor that is part of the sample carrier. The readout of the pressure sensor can be connected to a controller, for example, through a vacuum feedthrough of the glove box, or directly to a controller suitable for operating in an airless (e.g., argon) environment in the glove box.

[0043] The compression applied to the sample on the sample carrier in the glove box can be adjusted during installation and can be done in a variety of ways. As an example, one or a combination of the following approaches can be used, including adding a spacer between the sample and the support member. With reference to system 200 (although these are also applicable to any other disclosed examples), such spacers can be added between sample 202 and the first support portion 220 and / or the second support portion 222, or between other components along the arrangement of components of sample carrier 204. In some examples, the thickness of an element of the arrangement of components of sample carrier 204 can be adjusted, for example, using an adjustable screw in one or both of the first support portion 220 and the second support portion 222, thereby causing compression of sample 202. In other examples, one or more resilient members (such as springs, spring washers, elastic materials, rubber, etc.) can be added to the arrangement of components of sample carrier 204. In still other examples, the positioning of one or more elements of the arrangement of components of the sample carrier can be adjusted relative to base 208. For example, the positioning of the first support portion 220 and / or the second support portion 222 can be adjusted to compress the distance between the samples 202, such as in a typical bench vise arrangement.

[0044] In many examples, the compression regulated in this manner (such as within a glove box) can be maintained during transfer using a compression actuator, for example, a power source for an airless transfer container utilizing an electrically-based compression actuator (such as a piezoelectric transducer) coupled to the sample carrier, or more commonly utilizing mechanical components (such as the aforementioned spacers, vises, etc.). The mechanically applied compression can typically be passive, so that the battery sample can be held together during transport, and additional or different compressive forces applied by an electrical compression actuator (such as a piezoelectric transducer) can be applied after the sample carrier is engaged with the SEM stage. In many examples, it may be advantageous to transfer the SSB in a charged state, as the increased thickness in the charged state will itself maintain some compression during transport. Subsequent discharge in the SEM can result in a corresponding contraction of the SSB sample, which can then be absorbed by the electrically-operated compression transducer in the SEM.

[0045] In the selected method example 700, at 702, a battery sample can be placed in a holder of a sample carrier and slightly compressed (e.g., to approximately 1 MPa). In examples where the battery is not sealed in a pouch or button cell, such placement is typically performed in a glove box. At 704, in the case of a battery packaged such as a button cell or pouch cell, a portion of a cover including a portion of the battery is removed to obtain a cross-section that can be imaged in an SEM. Typically, such steps are performed in a glove box under argon. At 706, an airless transfer device connected to the glove box and a sample carrier loaded with the battery sample are loaded into the airless transfer device. At 708, the battery sample in the airless transfer device is moved to a wide ion beam polisher to flatten and polish the cross-section of the sample. For example, the airless transfer device can connect the chamber input to the wide ion beam polisher, and the sample carrier can be transferred to the chamber under controlled vacuum / airless conditions. At 710, once the sample carrier holding the battery sample is transferred under airless conditions (e.g., under argon), it can be transferred to a SEM (e.g., FIB-SEM, TriBeam, etc.) using an airless transfer device. At 712, a smooth, polished cross-section of the sample is obtained using a FIB and / or laser. At 714, in-situ electrical testing of the battery sample can be performed in the SEM along with SEM imaging and, optionally, FIB imaging. This in-situ electrical testing can be performed simultaneously or separately.

[0046] In some examples, 708 can be skipped and the sample carrier can be moved directly from the glove box to the SEM (or FIB / laser system, etc.). In other examples, 712 can be skipped entirely. In selected examples, where the battery surface is already in an acceptable state in the glove box (e.g., where the battery surface has been properly cross-sectioned and polished from a previous experiment), 708 and 712 can be skipped. In some examples, 708, 710, 712, or a combination thereof may be performed after 714 where more or improved polishing is required at a later time during SEM analysis (e.g., before / after electrical testing in the SEM). In many examples of method 700, the battery sample can remain in the same sample carrier throughout the entire process. In other examples, different sample carriers can be used for selected steps, e.g., where BIB polishing may require different mounts. In such examples, the sample can be mounted to a dedicated BIB sample carrier in the glove box before and after BIB polishing at 708.

[0047] General considerations

[0048] As used in this application and the claims, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. Additionally, the term "comprising" means "including." Furthermore, the term "coupled" does not exclude the presence of intervening elements between the coupled items.

[0049] The systems, devices, and methods described herein should not be construed as limiting in any way. Rather, the present disclosure relates to all novel and non-obvious features and aspects of the various disclosed embodiments, individually and in various combinations and subcombinations thereof. The disclosed systems, methods, and devices are not limited to any particular aspect or feature or combination thereof, nor do the disclosed systems, methods, and devices require any one or more specific advantages or problems to be solved. Any theory of operation is provided for ease of explanation, but the disclosed systems, methods, and devices are not limited to such theory of operation.

[0050] Although the operations of some of the disclosed methods are described in a particular sequential order for ease of presentation, it should be understood that this description includes rearrangement unless specific language described below requires a particular order. For example, the operations described in sequence may be rearranged or performed simultaneously in some cases. In addition, for simplicity, the accompanying drawings may not show the various ways in which the disclosed systems, methods, and devices can be used in conjunction with other systems, methods, and devices. Additionally, this description sometimes uses terms like "produce" and "provide" to describe the disclosed methods. These terms are high-level abstractions of the actual operations performed. The actual operations corresponding to these terms will vary depending on the specific implementation and can be easily discerned by those skilled in the art.

[0051] In some instances, values, procedures, or devices are referred to as "lowest," "optimal," "minimum," etc. It should be understood that such descriptions are intended to indicate that choices may be made among many functional alternatives used, and that such choices are not necessarily better, lesser, or otherwise preferred over other choices.

[0052] The principles of the disclosed technology have been described and illustrated with reference to the illustrated embodiments, and it will be appreciated that the illustrated embodiments may be modified in arrangement and detail without departing from such principles. For example, elements of the illustrated embodiments illustrated in software may be implemented in hardware, and vice versa. In addition, the techniques from any example may be combined with the techniques described in any one or more of the other examples. It will be understood that the procedures and functions such as those described with reference to the illustrated examples may be implemented in a single hardware or software module, or that separate modules may be provided. The above specific arrangements are provided for ease of description, and other arrangements may be used.

[0053] Additional Embodiments of the Disclosed Technology

[0054] Example 1. A device comprising: a sample carrier, the sample carrier comprising a base member and a sample support assembly connected to the base member, wherein the sample support assembly comprises a bracket, the bracket having a first bracket portion and a second bracket portion relative to each other, the first bracket portion and the second bracket portion being configured to compress the sample within a bracket receiving portion, wherein the base member is configured to engage a sample stage within a microscope chamber.

[0055] Example 2. An apparatus according to Example 1, wherein the base member includes a sliding member, the sliding member being configured to slidably engage the sample stage, wherein the sliding member includes a stop member, the stop member causing the sample stage to stop at a slidably engageable position within the microscope chamber.

[0056] Embodiment 3. An apparatus according to any one of embodiments 1 to 2, wherein each of the first support portion and the second support portion includes a first support electrical contact and a second support electrical contact, respectively, and the first support electrical contact and the second support electrical contact face the sample to engage the corresponding sample electrode.

[0057] Embodiment 4. The apparatus of any one of embodiments 1 to 3, wherein the first support portion comprises a compression actuator that applies a compressive force to the sample.

[0058] Embodiment 5. The apparatus of embodiment 4, wherein the compression actuator is a piezoelectric actuator.

[0059] Embodiment 6. The apparatus of any one of embodiments 1 to 5, wherein the first support portion and the second support portion comprise vises.

[0060] Embodiment 7. An apparatus according to any one of embodiments 1 to 6, wherein the sample carrier includes an electrical coupling portion, and the electrical coupling portion is configured to be electrically connected to the sample stage when the base member is engaged with the sample stage within the microscope chamber.

[0061] Embodiment 8. The apparatus of embodiment 7, wherein the electrical coupling to the sample stage is achieved by a slidable contact between a contact surface of the electrical engagement portion and a corresponding mating contact surface of the sample stage.

[0062] Embodiment 9. The apparatus of Embodiment 7, wherein the electrical engagement portion comprises an engagement contact pin or a receiving aperture configured to provide the electrical connection to the sample stage.

[0063] Embodiment 10. The apparatus of any one of Embodiments 7 to 9, wherein the sample carrier comprises at least one electrically conductive path electrically coupling at least a portion of the first support portion to the electrical engagement portion.

[0064] Embodiment 11. The apparatus of any one of embodiments 7 to 9, wherein the sample carrier comprises:

[0065] a first conductive path of the first bracket portion, the first conductive path electrically coupling the first bracket electrical contact to the electrical engagement portion;

[0066] a second conductive path of the first bracket portion, the second conductive path electrically coupling the compression actuator to the electrical engagement portion; and

[0067] The second bracket portion includes a first conductive path electrically coupling the second bracket electrical contact to the electrical engagement portion.

[0068] Embodiment 12. The apparatus of any one of Embodiments 10-11, wherein at least one of the conductive paths is coupled from the sample support assembly to the electrical engagement portion through the base member.

[0069] Embodiment 13. An apparatus according to any one of embodiments 10 to 12, wherein the electrical engagement portion is located at the stop member so that when the sample carrier is in the engaged position, at least one of the conductive paths is electrically connected to the sample stage through the stop member.

[0070] Embodiment 14. The apparatus of any one of Embodiments 1 to 13, wherein the second bracket portion is fixed relative to the base member.

[0071] Embodiment 15. The apparatus of any one of Embodiments 1 to 14, wherein the first support portion and the second support portion are configured to hold a button cell battery or a solid-state battery for testing within the microscope chamber.

[0072] Embodiment 16. The apparatus of embodiment 15, wherein the microscope chamber is a SEM chamber, a FIB chamber, a FIB-SEM chamber, a laser and SEM chamber, or a triple beam SEM / PFIB / laser microscope chamber.

[0073] Embodiment 17. A device comprising:

[0074] A sample carrier receiver, the sample carrier receiver comprising a support member having a base member and a receiving portion, the base member being coupled to a stage within a microscope chamber, the receiving portion being coupled to the base member, wherein the receiving portion comprises a sliding mount extending at an oblique angle relative to the base member to receive and secure the sample carrier relative to the sample stage within the microscope chamber by slidable engagement with the sliding mount; and wherein the receiving portion comprises an electrical engagement portion coupled to an electrical engagement portion of the sample carrier to provide an electrically conductive path from the sample carrier through the stage.

[0075] Embodiment 18. The apparatus of embodiment 17, further comprising the apparatus of any one of embodiments 1 to 16.

[0076] Example 19. A method comprising:

[0077] engaging an airless transfer container with an airless transfer container transfer port of a vacuum chamber of a microscope, wherein the airless transfer container stores a sample carrier;

[0078] inserting the sample carrier from the airless transfer container into the microscope vacuum chamber by moving the sample carrier into a sample carrier receptacle mounted on a sample stage located in the vacuum chamber; and

[0079] The electrical connection portion on the sample carrier and the electrical connection portion on the sample carrier receiver are electrically connected.

[0080] Embodiment 20. The method of embodiment 19, further comprising: before engaging the airless transfer container with the airless transfer container transfer port of the microscope vacuum chamber:

[0081] placing a battery sample on the sample stage in a glove box, and compressing the battery sample with the sample mounted on the sample stage;

[0082] mechanically treating the sample in the glove box to remove a portion of a cover of the sample;

[0083] The mechanically processed sample is transferred into the airless transfer container and then transferred into a broad ion beam (BIB) polisher;

[0084] polishing the sample supported by the sample stage with a broad ion beam in the broad ion beam (BIB) polisher; and

[0085] The BIB-treated and mechanically processed samples were transferred to the air-free transfer container.

[0086] Example 21. A method according to any one of Examples 19 to 20, wherein a compression force is applied to the sample supported by the sample carrier by a compression actuator during insertion of the sample carrier from the airless transfer container into the vacuum chamber of the microscope, and / or during movement of the airless transfer container away from the chamber and / or during storage of the airless transfer container.

[0087] Example 22. A method comprising: securing a sample carrier to a sample stage within a microscope chamber, wherein the sample carrier comprises a sliding member and a sample support assembly coupled to the sliding member, wherein the sample support assembly comprises a bracket having a first bracket portion and a second bracket portion relative to each other, the first bracket portion and the second bracket portion being configured to compress the sample within a bracket receiving portion, wherein the securing comprises: slidably engaging the sliding member to a sample carrier receiver coupled to the sample stage, and electrically coupling the sample carrier and corresponding electrical coupling portions of the sample carrier receiver; and charging and / or discharging the sample at least partially via the electrical coupling.

[0088] Embodiment 23. The method of embodiment 22, further comprising varying a compressive force applied to the sample during the charging and / or discharging at least in part through the electrical coupling.

[0089] In view of the many possible embodiments to which the principles of the disclosed technology may be applied, it should be recognized that the illustrated embodiments are merely representative examples and should not be considered to limit the scope of the present disclosure. The alternatives specifically set forth in these sections are merely exemplary and do not constitute all possible alternatives to the embodiments described herein. For example, the various components of the systems described herein may be combined in function and use. We therefore claim protection for all that falls within the scope of the appended claims.

Claims

1. A device, comprising: A sample carrier comprising a base member and a sample support assembly coupled to the base member, wherein the sample support assembly comprises a bracket having opposing first and second bracket portions configured to compress a sample within a bracket receiving portion, wherein the base member is configured to engage a sample stage within a microscope chamber.

2. The apparatus of claim 1 , wherein the base member comprises a sliding member configured to slidably engage the sample stage, wherein the sliding member comprises a stopper that stops the sample stage at a slidably engageable position within the microscope chamber.

3. The apparatus of claim 1 , wherein each of the first and second support portions comprises a first and second support electrical contact, respectively, the first and second support electrical contacts facing the sample to engage corresponding sample electrodes.

4. The apparatus of claim 3, wherein the first support portion comprises a compression actuator that applies a compressive force to the sample.

5. The apparatus of claim 4, wherein the compression actuator is a piezoelectric actuator.

6. The apparatus of claim 1, wherein the first bracket portion and the second bracket portion comprise vises.

7. The apparatus of claim 4, wherein the sample carrier includes an electrical engagement portion configured to electrically couple to the sample stage when the base member is engaged with the sample stage within the microscope chamber.

8. The apparatus of claim 7, wherein the electrical coupling to the sample stage is achieved by a slidable contact between a contact surface of the electrical engagement portion and a corresponding mating contact surface of the sample stage.

9. The apparatus of claim 7, wherein the electrical engagement portion comprises an engagement contact pin or a receiving hole configured to provide the electrical connection to the sample stage.

10. The apparatus of claim 7, wherein the sample carrier comprises at least one electrically conductive path electrically coupling at least a portion of the first support portion to the electrical engagement portion.

11. The apparatus according to claim 7, wherein the sample carrier comprises: a first conductive path of the first bracket portion, the first conductive path electrically coupling the first bracket electrical contact to the electrical engagement portion; a second conductive path of the first bracket portion, the second conductive path electrically coupling the compression actuator to the electrical engagement portion; and The second bracket portion includes a first conductive path electrically coupling the second bracket electrical contact to the electrical engagement portion.

12. The apparatus of claim 10, wherein at least one of the conductive paths is coupled from the sample support assembly to the electrical engagement portion through the base member.

13. The apparatus of claim 10 , wherein the base member comprises a sliding member configured to slidably engage the sample stage, wherein the sliding member comprises a stopper that stops the sample stage at a slidably engageable position within the microscope chamber; and wherein the electrical engagement portion is located at the stopper so that when the sample stage is in the engaged position, at least one of the conductive paths is electrically coupled to the sample stage via the stopper.

14. The apparatus of claim 1, wherein the second bracket portion is fixed relative to the base member.

15. The apparatus of claim 1, wherein the first and second support portions are configured to hold a button cell battery or a solid-state battery for testing within the microscope chamber.

16. The apparatus of claim 15, wherein the microscope chamber is a SEM chamber, a FIB chamber, a FIB-SEM chamber, a laser and SEM chamber, or a triple beam SEM / PFIB / laser microscope chamber.

17. A device comprising: a specimen stage receiver comprising a support having a base member coupled to a stage within a microscope chamber and having a receiving portion coupled to the base member, wherein the receiving portion includes a slide mount extending at an oblique angle relative to the base member to receive and secure a specimen stage relative to the specimen stage within the microscope chamber via slidable engagement with the slide mount; Wherein the receiving portion includes an electrical engagement portion that couples to an electrical engagement portion of the sample carrier to provide an electrically conductive path from the sample carrier through the stage.

18. The apparatus according to claim 17, further comprising: A sample carrier comprising a base member and a sample support assembly coupled to the base member, wherein the sample support assembly comprises a bracket having opposing first and second bracket portions configured to compress a sample within a bracket receiving portion, wherein the base member is configured to engage a sample stage within a microscope chamber.

19. A method comprising: engaging an airless transfer container with an airless transfer container transfer port of a vacuum chamber of a microscope, wherein the airless transfer container stores a sample carrier; inserting the sample carrier from the airless transfer container into the microscope vacuum chamber by moving the sample carrier into a sample carrier receptacle mounted on a sample stage located in the vacuum chamber; as well as The electrical connection portion on the sample carrier and the electrical connection portion on the sample carrier receiver are electrically connected.

20. The method according to claim 19, further comprising: Prior to engaging the airless transfer container with the airless transfer container transfer port of the microscope vacuum chamber: placing a battery sample on the sample stage in a glove box, and compressing the battery sample with the sample mounted on the sample stage; mechanically treating the sample in the glove box to remove a portion of a cover of the sample; The mechanically processed sample is transferred into the airless transfer container and then transferred into a broad ion beam (BIB) polisher; polishing the sample supported by the sample stage with a broad ion beam in the broad ion beam (BIB) polisher; as well as The BIB-treated and mechanically processed samples were transferred to the air-free transfer container.

21. A method according to claim 19, wherein a compression force is applied to the sample supported by the sample carrier by a compression actuator during insertion of the sample carrier from the airless transfer container into the microscope vacuum chamber, and / or during movement of the airless transfer container out of the chamber and / or during storage of the airless transfer container.

22. A method comprising: securing a sample carrier to a sample stage within a microscope chamber, wherein the sample carrier comprises a sliding member and a sample support assembly coupled to the sliding member, wherein the sample support assembly comprises a bracket having opposing first and second bracket portions, the first and second bracket portions being configured to compress the sample within a bracket receiving portion, wherein the securing comprises: slidably engaging the sliding member to a sample carrier receiver coupled to the sample stage, and electrically coupling corresponding electrical engagement portions of the sample carrier and the sample carrier receiver; and The sample is charged and / or discharged at least in part through the electrical coupling.

23. The method of claim 22, further comprising varying a compressive force applied to the sample during the charging and / or discharging at least in part through the electrical coupling.

Images