Functionalized sleeve for sample holder

Abstract

Methods and systems are provided for a system for supporting a sample. In one embodiment, a system includes: a charged particle sample holder configured to hold a sample for analysis; and a functionalized sleeve configured to receive the charged particle sample holder into an opening extending along an axis of the functionalized sleeve. When inserted, the functionalized sleeve encloses at least a portion of the charged particle sample holder. The functionalized sleeve includes one or more extensions disposed along the top or bottom of the sample, the one or more extensions including a stimulation component and / or a detection component.

Description

Technical Field

[0001] This disclosure relates throughout to methods and systems for connecting a transmission electron microscope (TEM) sample holder to a scientific instrument. Specifically, this disclosure relates to a sleeve for a sample holder that provides functionality for operations to be performed at the sample holder. Background Technology

[0002] Transmission electron microscopy (TEM) sample holders may have specific sizes (e.g., diameters) depending on their manufacturer. This can limit the use of a given sample holder to a specific scientific instrument (e.g., a TEM system), which may necessitate access to multiple sample holders to allow samples to be analyzed by different TEM systems. Furthermore, while sample holders may be movable when coupled to a scientific instrument to allow for repositioning of the corresponding sample within the instrument, they can also facilitate any additional actions or manipulations. Therefore, it is desirable for TEM sample holders to be adaptable to use with different TEM platforms and to provide functional capabilities at the sample holder location to enhance sample analysis and / or processing. Summary of the Invention

[0003] In at least one embodiment, a system includes: a charged particle sample holder configured to hold a sample for analysis; and a functionalized sleeve configured to receive the charged particle sample holder into an opening extending along an axis of the functionalized sleeve. Upon insertion, the functionalized sleeve encloses at least a portion of the charged particle sample holder. Furthermore, the functionalized sleeve includes one or more extensions disposed along the top or bottom of the sample, the one or more extensions including a stimulation element and / or a detection element.

[0004] In another embodiment, a functionalized sleeve for a transmission electron microscope (TEM) sample holder includes a cylindrical housing, one or more extensions extending from a first end of the cylindrical housing, and sensing and / or detection components coupled to the one or more extensions. Furthermore, the functionalized sleeve includes one or more ports in the cylindrical housing configured to allow a feedthrough of the sensing and / or detection components to pass through.

[0005] In yet another embodiment, a method of using a sample support device including a functionalized sleeve includes: loading a sample onto a sample holder of the sample support device; positioning the sample in the path of a charged particle beam; and activating a stimulation element and / or a detection element supported by the functionalized sleeve. The method also includes acquiring data from the sample when the sample is irradiated by the charged particle beam. Attached Figure Description

[0006] To facilitate the identification of any particular element or action in the discussion, one or more of the largest significant digits in the reference numerals refer to the drawing number in which the element is first introduced.

[0007] Figure 1 A cross-sectional view of a functionalized sleeve for a TEM sample holder according to one embodiment is shown.

[0008] Figure 2 A cross-sectional view of a sample support device according to one embodiment is shown, the sample support device including a sample holder coupled to it. Figure 1 Functionalized sleeve.

[0009] Figure 3 A portion of a sample support device including a functionalized sleeve, according to one embodiment, is shown.

[0010] Figure 4 A portion of a sample support device including a functionalized sleeve, according to one embodiment, is shown.

[0011] Figure 5 A portion of a sample support device including a functionalized sleeve, according to one embodiment, is shown.

[0012] Figure 6 An embodiment is shown. Figure 3 It is part of a functionalized sleeve.

[0013] Figure 7 An embodiment is shown. Figure 3 A functionalized sleeve, which is connected to a coupling mechanism for aligning the functionalized sleeve with a scientific instrument.

[0014] Figure 8 The control mechanism connected to the scientific instrument is shown according to one embodiment. Figure 3 The sample support device.

[0015] Figure 9 A portion of a sample support device with a functionalized sleeve according to one embodiment is shown, the functionalized sleeve including a vacuum transfer fitting in an open position.

[0016] Figure 10 The closed position is shown according to one embodiment. Figure 9 Vacuum transfer accessories.

[0017] Figure 11 A scientific instrument using a sample support device with a functionalized sleeve is shown according to one embodiment.

[0018] Figure 12A method for using a sample support device with a functionalized sleeve, according to one embodiment, is shown. Detailed Implementation

[0019] The following description relates to systems and methods for increasing the adaptability and functionality of TEM sample holders. This allows for greater versatility of the sample holder while maintaining the integrity of the associated sample supported by the sample holder.

[0020] The sample is supported within the TEM system by a TEM sample holder (hereinafter referred to as the sample holder). The sample holder holds the sample within the TEM tube so that the sample is irradiated by a beam of charged particles (e.g., an electron beam), thereby allowing the acquisition of physical and chemical information from the sample. In some cases, the sample holder may have limited capabilities, such as the permissible amount of movement, to adjust the position of the sample within the TEM tube. Such movement may include, for example, tilting the sample relative to the electron beam, and translating the sample into and out of the TEM tube. However, moving the sample into and out of the TEM tube via the sample holder may expose the sample to air, at least briefly.

[0021] Furthermore, the sample holder may lack the structure or configuration that allows for the performance of additional sample-related tasks or operations while the sample is supported (e.g., engaged) by the sample holder. For example, the sample holder may lack any openings that allow feedthroughs (e.g., connectors, links, conduits, etc. for electrical, mechanical, and / or material transport) to facilitate processes and operations performed at the sample. To allow such handling of the sample, it may be necessary to remove the sample from the TEM tube, which prolongs the workflow and may expose the sample to air and / or contaminants.

[0022] Furthermore, sample holders can be manufactured with geometries and dimensions specific to a particular TEM platform. For example, a sample holder produced by a particular manufacturer may only fit a TEM tube manufactured by that manufacturer. Therefore, users may need to obtain sample holders for each TEM platform they wish to use to analyze samples, which can be expensive and impractical.

[0023] In at least one embodiment, as described herein, a sample holder may be coupled to a functionalized sleeve that circumferentially surrounds at least a portion of the sample holder. For example, the sample holder may be inserted into the functionalized sleeve to form a sample support device. The sample support device may be inserted into a TEM holder such that the sample holder will securely hold the sample in the proper position within the TEM holder, even if the sample holder has geometry and / or dimensions incompatible with the receiving port of the TEM tube. For example, the functionalized sleeve may be used most effectively when the diameter of the sample holder is too small to remain stable within the receiving port of the TEM tube. By coupling the sample holder to the functionalized sleeve, the diameter of the resulting sample support device can be adapted for use with the TEM tube. Furthermore, the functionalized sleeve may include a feedthrough that allows the delivery and / or retrieval of control signals and / or electrical signals, as well as material, to or from components coupled to the functionalized sleeve.

[0024] As an example, a functionalized sleeve can be configured to provide functionality within a sample support device, including stimulation functions (e.g., gas stimulation, light stimulation, electrical stimulation, and / or magnetic stimulation), sensing functions (e.g., mirror apertures, phase plates, detectors, etc.), and environmental functions (e.g., gas injection, vacuum, cryogenic conditions, etc.). This functionality can be achieved at the sample end of the device from a position above, below, or both above and below the sample plane of the sample support device. Therefore, data collected from the sample can be enhanced while reducing the sample's exposure to undesirable media (e.g., air and other contaminants).

[0025] By pairing TEM sample holders with functionalized sleeves, users experience greater freedom in using available sample holders for available TEM platforms. For example, constraints on the connection between a particular sample holder and an available TEM platform can be reduced (e.g., having a common manufacturer), allowing sample holders with different geometries and / or sizes to be compatible with a given TEM system. Therefore, users can select TEM tubes based on desired characteristics, unrestricted by compatibility limitations between available sample holders and TEM tubes. Furthermore, in-situ and custom experiments, such as those utilizing heating, cooling, and detection, can be performed via functionalized sleeves, increasing the quantity and diversity of data obtainable from the sample.

[0026] Other benefits offered by the functionalized sample holder sleeves described herein include: economic advantages in use by allowing users to choose between different TEM tube suppliers without sacrificing sample holder capabilities; the ability to maintain samples in an inert environment even during sample transfer; and the ability to facilitate the design of new experiments by utilizing the multimodal capabilities provided by the sleeve. The technical effects of utilizing functionalized sample holder sleeves include allowing for more robust experimental opportunities for scientific and engineering advancements. Functionalized sleeves provide capabilities for multiple sample manipulation and data collection modalities while allowing backward compatibility with older sample holders. Exemplary configurations of functionalized sample holder sleeves are described in... Figures 1 to 10 It is described in the text and further described below.

[0027] Figure 1 A cross-sectional view of an example functionalized sample holder sleeve 100 (hereinafter referred to as sleeve 100 for simplicity) is shown. Sleeve 100 has a sample end 102 and an external end 104. In at least one embodiment, when sleeve 100 is inserted into a TEM tube and aligned with the electron beam of the TEM tube, sample end 102 is positioned inside the TEM tube, while external end 104 may extend outside the tube. Each of sample end 102 and external end 104 includes a feedthrough port 106, which may include feedthrough elements, such as interfaces, openings, fittings, etc., to accommodate conduits, wires, sensors, and other functional feedthrough elements through which they pass. Furthermore, feedthrough port 106 may allow feedthrough elements to connect sample end 102 of sleeve 100 to devices, components, and / or devices outside sleeve 100 and / or outside the TEM tube. In some examples, feedthrough elements may be used to provide connectivity (e.g., electronic and / or mechanical) to functionalized features or mechanisms at sample end 102 of sleeve 100.

[0028] The sample end 102 may include a first opening 108, and the outer end 104 may include a second opening 110. The first opening 108 allows the sample end of the sample holder to protrude through it, and the second opening 110 allows the outer end of the sample holder to protrude through it (e.g., as shown in the image). Figure 2 (As shown). The first opening 108 and the second opening 110 may define (e.g., along the x-direction) the end of an internal channel 118 extending through the length of the sleeve 100. In at least one example, the z-direction may be parallel to the beam emission axis of the TEM electron beam.

[0029] The sleeve 100 may also include alignment retainers 112 positioned along both the outer surface 114 and the inner surface 116 of the sleeve 100. The alignment retainer 112 along the outer surface 114 is alignable to the sleeve 100 relative to the TEM barrel, and the alignment retainer 112 along the inner surface 116 is alignable to the sleeve 100 relative to the TEM sample holder. For example, the alignment retainer 112 may slide into grooves or recesses in the surfaces of the TEM barrel and the TEM sample holder such that once the alignment retainer 112 engages with the corresponding groove or recess, the sleeve 100 is kept aligned relative to the TEM barrel and / or the TEM sample holder is kept aligned relative to the sleeve 100. It should be understood that... Figures 3 to 10 The implementation of the functionalized sleeve shown and further described below may include similar... Figure 1 The alignment fastener 112 is not shown for the sake of simplicity.

[0030] Figure 2 The image shows a sample support device 200 including a sample holder 202 coupled to a sleeve 100 such that the sample holder 202 and the sleeve 100 are coaxial (e.g., the axis of the sample holder 202 along its length is aligned with the axis of the sleeve 100 along its length, where the length is defined in the x-direction). In at least one embodiment, the sleeve 100 may be configured to receive the sample holder 202. For example, the sample holder 202 may be inserted through a second opening 110 of the sleeve 100 and continue insertion until the sample holder 202 contacts a portion of the inner surface 116 of the sleeve 100 at the sample end 102. As an example, a portion 204 of the sample holder 202, where the diameter (e.g., defined in the z-direction) widens, may abut the inner surface 116 of the sleeve 100. This prevents further translation of the sample holder 202 relative to the sleeve 100 toward the sample end 102 of the sleeve 100.

[0031] The sample end 206 of the sample holder 202 may protrude or extend outward from the first opening 108. At the sample end 206, a sample (e.g., a TEM sample) may be placed in the sample holder 202, which maintains the sample in a stationary position relative to the sample holder 202 and the TEM tube. When the sample support device 200 is inserted into the TEM tube, the sample may be positioned in the path of the electron beam emitted by the electron source of the TEM tube. In at least one embodiment, the sample end 206 of the sample holder 202 may be maintained under low pressure (e.g., vacuum) during, for example, sample preparation, sample transfer to the TEM tube, and / or when the sample is inserted into the TEM tube.

[0032] At the outer end 208 of the sample holder 202, the sample holder 202 may protrude or extend outward from the outer end 104 of the sleeve 100. In at least one embodiment, both the outer end 104 of the sleeve 100 and the outer end 208 of the sample holder 202 are outside the TEM tube when the sample support device 200 is inserted into the TEM tube. This allows the sample holder 202 to be adjusted and manipulated when studying samples using the TEM tube.

[0033] like Figure 2 As shown, the inner and outer diameters of the sleeve 100 (where the diameter is defined along the z-direction) are both larger than the diameter of the sample holder 202 along its length or axis. At least a portion of the sample holder 202 can be circumferentially surrounded or enclosed by the sleeve 100. In cases where the sample holder 202 has a diameter too narrow for the receiving port of the TEM tube, the sample holder 202 can be coupled to the sleeve 100 and inserted into the TEM tube as a sample support 200, wherein the sample support 200 has an outer diameter compatible with the receiving port of the TEM tube. When the diameter of the sample holder 202 is compatible with the receiving port of the TEM tube, the sleeve 100 can be omitted, and the sample holder 202 can be inserted into the TEM tube without using the sleeve 100.

[0034] As described above, the feedthrough port 106 of the sleeve 100 can endow the sleeve 100 with various functions for use with a sample supported by the sample holder 202. For example, the feedthrough port 106 can support stimulation components, including but not limited to heating components, cooling components, gas supplies directed toward the sample, power supplies, magnetic sources, and / or light sources. The feedthrough port 106 can also support one or more detection components, including but not limited to secondary electron detectors, backscattered electron detectors, mirrors for light collection, dedicated apertures, phase plates, optical detectors, and / or X-ray detectors, as well as any additional components for various stimulation or detection / sensing schemes that can be deployed when probing the sample with an electron beam. As described herein, a variety of experimental conditions and experimental types can be expanded by utilizing the functionalized sleeve with the feedthrough port.

[0035] In some examples, the functionalized sample sleeve of the sample support device may include one or more structural elements to support the integration of one or more functionalities into the sleeve, allowing the functionality to be applied to the sample. Figure 3 A first example of a sample support device 300 is depicted, which includes a functionalized sample holder sleeve 302 having such structural elements. The sample support device 300 may be... Figure 2An embodiment of the sample support device 200 is described. A sample holder 304 is coupled to a sleeve 302. The sample holder 304 includes a sample ring 303 in which a sample (e.g., a TEM grid) can be placed for study using a TEM tube. In at least one embodiment, the sleeve 302 is a cylindrical shell or tube whose length relative to the x-direction is greater than the diameter 301 of the sleeve 302.

[0036] like Figure 3 As shown, the sleeve 302 includes an extension 306 positioned below (e.g., relative to the z-direction) the sample end 308 of the sample holder 304, which protrudes beyond the sleeve 302. For example, the sample end 308 of the sample holder 304 may be accessible from an opening at the sample end 310 of the sleeve 302 (e.g., similar to...). Figure 1 The first opening 108 extends in the x-direction. The extension 306 may extend parallel to the sample end 308 of the sample holder 304 from the sample end 310 of the sleeve 302. In one example, as... Figure 3 As shown, the length of the extension 306 along the x-direction matches the amount by which the sample end 308 of the sample holder 304 also protrudes from the sleeve 302 along the x-direction. However, in other examples, the length of the extension 306 may not be equal to the protrusion of the sample end 308 of the sample holder 304 from the sleeve 302. For example, the length of the extension 306 may be greater than or less than the protrusion of the sample end 308 of the sample holder 304. Similar variability applies to... Figure 4 and Figure 5 The extension shown.

[0037] Furthermore, when the sample is located within the sample ring 303, the extension 306 is arranged below the sample relative to the direction of the beam emitted by the electron source (as indicated by arrow 305). The extension 306 is thus positioned along the bottom of the sample. The extension 306 may be a protrusion coupled to and extending outward from the sample end 310 of the sleeve 302 along the x-axis. In at least one embodiment, the extension 306 may include a hole 312 aligned with the central opening of the sample ring 303, such as... Figure 6 This is shown more clearly in the text.

[0038] Figure 6The sleeve 302 is depicted without a sample holder 304 attached to it. The aperture 312 may be a through-hole extending completely through the thickness of the extension 306 (e.g., defined along the z-axis). The aperture 312 may be aligned with the central opening of the sample ring 303 such that an electron beam transmitted through the sample can pass through the aperture 312 unaffected and unobstructed by the extension 306. The extension 306 may support one or more functional components (not shown), including stimulation and detection components, wherein the functional components may be arranged around the aperture 312 on the extension 306. Alternatively, if arranged in the path of the electron beam, the functional components may also include apertures for allowing the beam to pass through them.

[0039] Return to Figure 3 The sleeve 302 may also include one or more feed ports 314. The feed ports 314 allow connections between functional components and equipment located outside the sample support assembly 300 to pass through the sleeve 302. It should be understood that... Figures 3 to 10 The size, shape, and relative positioning of the feed port and other components of the sample support device depicted are non-limiting examples and may be varied without departing from the scope of this disclosure.

[0040] exist Figure 4 The image shows a second example of a sample support device 400, which includes a functionalized sample holder sleeve 402 coupled to and surrounding at least a portion of a sample holder 404. The sample support device 400 may be... Figure 2 An embodiment of the sample support device 200, and similar to... Figure 3 The sample support device 300 differs in that it supports the positioning of structural elements that integrate functionality into a sleeve 402. The sleeve 402 includes an extension 406 positioned above (e.g., relative to the z-direction) the sample end 408 of the sample holder 404 and extending from the sample end 410 of the sleeve 402. The extension 406 thus arranges along the top of the sample supported by the sample holder 404. The sample end 408 has an opening at the sample end 410 of the sleeve 402 (e.g., similar to...). Figure 1 The first opening 108) protrudes. The sample end 408 of the sample holder 404 includes a sample ring 403 to support the sample. In at least one embodiment, the extension 406 includes a hole 412 aligned with the central opening of the sample ring 403 (in Figure 4 (obscured in the middle), such as Figure 3 The apertures 312 and 406 allow an electron beam to pass through and strike the sample. Various functional components (not shown), including stimulation and detection components, may be arranged along the extension 406 and pointed toward the sample. If positioned in the path of the electron beam, the functional components may include apertures to accommodate the beam passage passing through them.

[0041] Sleeve 402 may also include one or more feed ports 414. Feed ports 414 allow connections between functional components and equipment located outside sample support 400 to pass through sleeve 402.

[0042] A third example of a sample support device 500 is shown, which includes a sample holder 504 to which a functionalized sample holder sleeve 502 is coupled. The sample support device 500 may be... Figure 2 An embodiment of the sample support device 200, and can be combined with Figure 3 and Figure 4 The sample support devices 300 and 400 have structural elements. For example, sleeve 502 includes a set of extensions 506 projecting outward from the sample end 510 of sleeve 502 in the x-direction. These extensions 506 include components similar to... Figure 4 The upper extension 506a of the extension 406 and similar to Figure 3 The lower extension 506b of the extension 306. The upper extension 506a may extend above the sample end 508 of the sample holder 504, and the lower extension 506b may extend below the sample end 508 of the sample holder 504, wherein the references to upper and lower are oriented relative to the z-direction.

[0043] The sample end 508 of the sample holder 504 can be similar to Figure 3 The sample end 308 of the sample holder 304 or Figure 4 The sample end 408 of the sample holder 404. For example, although in Figure 5 Not visible in the image, but the sample end 508 of the sample holder 504 may include a sample ring, such as... Figure 3 Sample ring 303 or Figure 4 The sample ring 403. Each extension in the set of extensions 506 may include a hole 512 aligned with the central opening of the sample ring. By arranging extensions above and below the sample end 508 of the sample holder 504, functional components, including stimulation and detection components, can be incorporated into the sample support 500, close to the sample, without interfering with beam transport. Feedthroughs of the functional components may pass through feedthrough ports 514 of the sleeve 502 to provide functionality to the functional components.

[0044] exist Figure 7 middle, Figure 3The outer end 702 of the sleeve 302 is shown to have a coupling mechanism 704. The coupling mechanism 704 may be arranged at the end of the sleeve 302 opposite to the sample end 310 of the sleeve 302. When the sleeve 302 is inserted into the receiving port of the TEM tube, the outer end 702 may protrude outside the TEM tube. The coupling mechanism 704 can be used to align and secure the sleeve 302 to the TEM tube. For example, the coupling mechanism 704 may engage a mechanism or structure at the TEM tube to hold a sample support device (e.g., Figure 3 The sample support device 300 is positioned at the desired alignment location relative to the electron beam and the internal components of the TEM tube. The engagement mechanism 704 may include one or more alignment posts 706 that slide into corresponding alignment holes in the TEM tube. The engagement mechanism 704 may also include one or more connectors 708 that provide electronic and fluid connections between the sample end 310 of the sleeve 302 and devices external to the sleeve 302.

[0045] Figure 8 The image shows a sleeve 302, a sample holder 304, and... Figure 7 The coupling mechanism 704 Figure 3 The sample support device 300 is connected to the control mechanism 802. The control mechanism 802 can be used to control components of a TEM system with a TEM tube into which the sample support device 300 is inserted. For example, the control mechanism 802 can allow the sample holder 304 to tilt, rotate, or otherwise reposition relative to the electron beam in three-dimensional space.

[0046] A control mechanism 802 may be coupled to the sample support 300 at a location adjacent to the engagement mechanism 704 along the outer end 804 of the sample holder 304. In at least one embodiment, the control mechanism 802 may abut and engage with the engagement mechanism 704 along the x-direction. As previously described, the outer end 804 of the sample holder 304 may protrude beyond the TEM tube when the sample support 300 is inserted into the TEM tube. In some examples, at least a portion of the control mechanism 802 may also protrude beyond the TEM tube. However, in other examples, the entire sample support 300 may alternatively be placed inside the loading lock cavity, such as during sample loading into the sample holder 304 and during sample storage when the sample is not being studied using the TEM tube. Furthermore, in at least some cases, the TEM tube may include a sample holder engagement member that completely encloses the sample support 300 when it is inserted into the TEM tube.

[0047] In at least one embodiment, the functionalized TEM sample holder sleeve can be used in conjunction with a sample holder that supports a sample to be maintained under low pressure (e.g., vacuum). Therefore, the sleeve may include structural elements for sealing a portion of the sample holder to maintain the low-pressure conditions. As an example, such as Figure 9 and Figure 10 As shown, the sample support device 900 may include a functionalized sleeve 902 with a vacuum transfer fitting 904. The vacuum transfer fitting 904 can seal the sample therein to isolate the sample from the surrounding environment around the sample support device 900.

[0048] Similar to Figures 3 to 5 and Figure 8 The sample holder depicted is coupled to a sleeve 902 and protrudes from the sample end 906 of the sleeve (e.g., along the x-direction). In at least one embodiment, in addition to the vacuum transfer fitting 904, the sleeve 902 may also include one or more extensions, such as Figures 3 to 8 The extension shown is illustrated. However, in other examples, sleeve 902 may include vacuum transfer fitting 904 without any additional extension. In such examples, at least a portion of vacuum transfer fitting 904 may be an extension of sleeve 902, having a... Figures 3 to 8 The extensions depicted in the image have different geometric structures.

[0049] Vacuum transfer accessory 904 Figure 9 It is shown as being in the open position, and in Figure 10 The middle part is shown as being in a closed position. For example... Figure 9 As shown, the vacuum transfer fitting 904 includes an inner portion 904a and an outer portion 904b. The inner portion 904a may be an extension coupled to and extending from the sample end 906 of the sleeve 902, and may be configured to surround the sample end of the sample holder. The inner portion 904a may have a box-like geometry (e.g., shaped as a rectangular prism or cube) and may include a hole 908 disposed in a face intersecting the z-direction of the inner portion 904a. The hole 908 may be aligned with a central opening of the sample ring of the sample holder to allow an electron beam to pass through the inner portion 904a. One or more functional structures (e.g., stimulation and / or detection components) may be coupled to the inner portion 904a, such as along the inner surface of the inner portion 904a, near the sample supported by the sample end of the sample holder.

[0050] The outer portion 904b of the vacuum transfer accessory 904 can be a cover that completely encloses the inner portion 904a when connected to and engaged with the sample end 906 of the sleeve 902. In other words, the outer portion 904b can cover both the inner portion 904a and the sample end of the sample holder. For example, as Figure 10As shown, the inner portion 904a of the vacuum transfer fitting 904 can be inserted into the inner cavity of the outer portion 904b. By pressing the edge of the outer portion 904b at its open end, so that the edge abuts and engages with the sample end 906 of the sleeve 902, the vacuum transfer fitting 904 can be adjusted to... Figure 10 The closed position depicted in the text.

[0051] In at least one embodiment, control signals can be provided to one or more mechanisms via sleeve 902 (such as via one or more feed ports 910) to facilitate... Figure 9 and Figure 10 The vacuum transfer accessory 904 is automatically adjusted between open and closed positions, as shown in the diagram. For example, when the sample support 900 is inserted into the TEM tube for sample exploration using an electron beam, the vacuum transfer accessory 904 can be adjusted to the open position. Before insertion into the TEM tube, a sample can be prepared in a sample preparation apparatus (such as, for example, a loading lock cavity) and loaded onto a sample holder. Within the sample preparation apparatus, when the sample is loaded into the sample support 900, the sample and the sample support 900 can be maintained under low pressure. As an example, the sample can be loaded under low-pressure conditions similar to the low-pressure environment of the TEM tube. Once the sample loading is complete, the vacuum transfer accessory 904 can be adjusted to the closed position, and the sample can be transferred to the TEM tube without exposing the TEM sample to environmental conditions. The vacuum transfer accessory 904 can only be adjusted to the open position in a suitable low-pressure and / or clean environment to maintain sample integrity.

[0052] Figure 11 An example of an environment is depicted, in which a functional sample holder sleeve, such as Figures 1 to 10 Any of the sleeves shown can be used in conjunction with a sample holder to allow for the study of the sample using a charged particle beam. Figure 3 The environment is a TEM system 1100, which includes an electron source section 1101 (including an electron source 1103), a TEM tube 1105 (including a sample section 1107, an objective probe forming lens 1108, an objective imaging lens 1109, and a projection optics system 1111), and a detector section 1110 (including, for example, one or more detectors 1115).

[0053] In short, the electron source section 1101 includes electronic devices configured to excite a charged particle source, which may include a high-voltage field emission source or other electron-emitting sources, such that an electron beam is formed and conducted through a vacuum into the TEM barrel 1105. The TEM barrel 1105 includes components for beam formation, including electromagnetic and / or electrostatic lenses and multiple apertures to control the properties of the electron beam. The TEM barrel 1105 includes sample section 1107 components, such as a condenser lens, objective lenses (e.g., objective probe forming lens 1108 and objective imaging lens 1109), a miniature condenser lens, and a sample support device 1120. The sample section 1107 accommodates a sample through which the electron beam can pass. The TEM barrel 1104 also includes projection optics system 1111 components, such as projector lenses, differential lenses and intermediate lenses, aberration correctors, deflectors, astigmatism reducers, etc., and corresponding apertures (e.g., selected area diffraction apertures).

[0054] In at least one embodiment, as described above, the sample support 1120 of sample section 1107 can be used to support the sample and maintain its position relative to the electron beam. At least a portion of the sample holder of the sample support 1120 may be circumferentially surrounded by a functionalized sleeve that provides functionality to allow various stimulation and detection components to be applied to the sample to acquire data. In some examples, in addition to or in place of one or more extensions supporting the stimulation and detection components, the functionalized sleeve may include a vacuum transfer fitting that can be used to encapsulate the sample during transfer of the sample support from another device (e.g., a sample preparation or loading device) to the TEM tube 105. This allows the sample to be shielded from contaminants, protected from contact with external objects, and / or maintained in a desired low-pressure environment.

[0055] Detector section 1110 includes one or more types of detectors, sensors, screens, and / or optics configured to generate images, spectra, and other data for use in sample imaging and / or microanalysis. For example, the detector may include a pixelated electronic detector, a secondary electronic detector, one or more cameras, an electron energy loss spectrometer, an energy-dispersive X-ray spectrometer, etc.

[0056] TEM system 1100 may be wirelessly or electrically connected to control system 1130 via hardwired connection. Control system 1130 may include one or more computing devices having one or more processors to control components of TEM system 1100. For example, control system 1130 may include one or more user interfaces to receive requests and other inputs from users. Control system 1130 may perform various tasks and operations in response to these requests and inputs. As an example, upon detecting that sample support 1120 has been inserted into TEM tube 1105, and in response to receiving a request to study a sample, control system 1130 may command the activation of an electron source to emit an electron beam having a target energy intensity, beam current, spot size, etc. Control system 1130 may also command the initiation and termination of data acquisition at detector 1115. In at least one embodiment, when sample support 1120 includes a vacuum transfer fitting, control system 1130 may send instructions to sample support 1120 to adjust the vacuum transfer fitting between an open position and a closed position. The control system 1130 may also include a memory (e.g., a non-transitory memory) to store executable instructions and other information, such as collected data.

[0057] Figure 12 An example of a method 1200 for using a sample support device in a charged particle system is shown, wherein the sample support device includes a functionalized sleeve. In at least one embodiment, the charged particle system may be Figure 11 The TEM system 1100. The sample support device can be similar to... Figures 2 to 5 or Figures 8 to 10 Any of the sample support devices shown in the sample support apparatus. At least a portion of method 1200 may be operated by a user or operator (e.g., manually), or via a control system (such as... Figure 11 The control system 1130) controls automated processes or combinations thereof to perform them. Figure 12 In this context, operations are each instantiated once in a specific order, but operations can be reordered and / or repeated as needed and as appropriate (e.g., different operations can be executed in parallel where appropriate).

[0058] It should be understood that in some cases, the use of a functionalized sleeve can be avoided, such as when the diameter of the TEM sample holder is similar to the inner diameter of the receiver port of the TEM system. For example, the difference between the inner diameter of the receiver port and the diameter of the TEM sample holder may be too small to accommodate the diameter increase caused by the connection of the sleeve to the sample holder. In such examples, a sample holder can be used without a sleeve, but the sample holder may not be able to support the functionality provided by the sleeve.

[0059] At 1202, the method includes preparing a sample for study and analysis using a charged particle beam. In at least one embodiment, preparing a sample for study allows probing of the sample by irradiating it with a charged particle beam (e.g., an electron beam) to collect data based on the interaction between the sample and the charged particle beam. For example, the data may include images, elemental composition, crystallographic information, morphology, electronic structure, chemical bonding information, and so on. Sample preparation may include operations as shown in 1204 to 1208.

[0060] In one example, sample preparation may optionally include attaching a functionalized sleeve to a sample holder at 1204. For example, the sleeve and sample holder may be placed in a sample preparation apparatus, and the sample holder may be inserted into the sleeve such that the sleeve circumferentially surrounds at least a portion of the sample holder along its length, wherein the sample end of the sample holder protrudes from the sample end of the sleeve. In at least one embodiment, the attachment such that one or more structural elements of the sleeve are positioned proximally to the sample end of the sample holder, wherein the one or more structural elements may be extensions supporting one or more functional components (including stimulation and detection components) (e.g., such as...). Figures 3 to 8 (As shown). In another embodiment, one or more structural elements may include vacuum transfer fittings (e.g., such as...). Figure 9 and Figure 10 (As shown), and this connection causes the sample end of the sample holder to be enclosed by the internal portion of the vacuum transfer fitting. The internal portion of the vacuum transfer fitting can similarly support the functional components. Furthermore, the sleeve may include an extension or one or more of the vacuum transfer fittings, wherein the extension or one or more of the vacuum transfer fittings can support the functional components.

[0061] Preparation of a sample for research may include loading the sample onto the sample holder of a sample support device at 1206. As an example, the sample support device and sample may be stored or placed within a sample preparation device. The sample may be placed on the sample end of the sample holder within the sample preparation device, such as on the sample ring of the sample holder. In other examples, the sample may be prepared outside the sample preparation device, for example, under ambient conditions.

[0062] Despite Figure 12 The connection between the sleeve and the sample holder is shown as being performed before the sample is loaded onto the sample holder; however, it should be understood that in some cases, the functionalized sleeve may alternatively be connected to the sample holder after the sample is loaded. For example, when the sleeve is as follows: Figure 3 and Figures 6 to 8In the configuration shown (where the sleeve includes an extension located below the sample ring of the sample holder), the sample can be loaded onto the sample holder before or after the sleeve is attached to the sample holder. In the sleeve configuration including an extension arranged above the sample ring (e.g., as shown...), Figure 4 and Figure 5 As shown), the sample can be loaded onto the sample ring before the sleeve is attached to the sample holder. Additionally, when the sleeve includes a vacuum transfer accessory (e.g., as shown...), Figure 9 and Figure 10 As shown, the sample can also be loaded onto the sample ring before the sleeve is connected to the sample holder.

[0063] Sample preparation may also optionally include adjusting the vacuum transfer fitting at 1208. For example, when the sleeve includes the vacuum transfer fitting, the fitting may initially be in the open position (e.g., as shown in the image) when the sample is loaded onto the sample holder within the sample preparation apparatus and the sleeve is attached to the sample holder. Figure 9 (As shown). During these operations, the sample preparation apparatus can maintain a low-pressure environment. This is achieved by adjusting the vacuum transfer fitting to the closed position (e.g., as shown). Figure 10 As shown, the low-pressure environment of the sample preparation device is maintained within the vacuum transfer fitting where the sample is located.

[0064] At 1210, method 1200 includes providing a sample to a charged particle system (e.g., a TEM tube for a TEM system). For example, a sample support device may be inserted into a receiving port of the TEM tube. In at least one embodiment, the sample support device may include a engagement mechanism, such as... Figure 7 The engagement mechanism 704 aligns the sample support device with the TEM tube. By inserting the sample support device into the TEM tube according to the engagement mechanism, the sample can be aligned with a beam of charged particles emitted by an electron source of the TEM tube. In at least one embodiment, when the sample support device includes a vacuum transfer accessory, the accessory can be adjusted to the open position once the sample is supplied to the charged particle system. However, in other examples, the vacuum transfer accessory can be adjusted to the open position during subsequent operations of method 1200 (e.g., during 1212 or 1214).

[0065] At 1212, method 1200 includes a functional component for activating the sleeve. For example, one or more stimulation components and / or one or more detection components coupled to the sleeve may be activated and / or excited via a feedthrough port through the sleeve. One or more stimulation components may be used to apply stimulation to the sample to, for example, promote a response at the sample that can be monitored using a TEM system. One or more detection components may be used to detect and / or monitor the progress or state of the stimulation provided by the one or more stimulation components (e.g., as feedback).

[0066] At 1214, method 1200 includes acquiring data from the sample. For example, when the sample is irradiated by an electron beam and optionally exposed to functionality provided by a functionalized sleeve, the detector of the TEM system may be instructed (e.g., by a control system) to collect information from the sample.

[0067] In one embodiment, a system includes: a charged particle sample holder configured to hold a sample for analysis; and a functionalized sleeve configured to receive the charged particle sample holder into an opening extending along an axis of the functionalized sleeve, such that, upon insertion, the functionalized sleeve encloses at least a portion of the charged particle sample holder, wherein the functionalized sleeve includes one or more extensions disposed along the top or bottom of the sample, the one or more extensions including a stimulation element and / or a detection element. In a first embodiment, the functionalized sleeve further includes a vacuum transfer fitting capable of covering the sample end of the charged particle sample holder. In another embodiment, including one or more embodiments of the preceding embodiments, the vacuum transfer fitting is adjustable between an open position and a closed position, wherein in the open position the sample is exposed to the environment surrounding the charged particle sample holder, and in the closed position the sample is sealed within the vacuum transfer fitting. In another embodiment including one or more embodiments of the preceding embodiments, the stimulation component includes one or more of a heating component, a cooling component, a gas supply portion guided toward the sample, a power source, a magnetic source, or a light source component. In another embodiment including one or more embodiments of the preceding embodiments, the detection component includes one or more of a secondary electron detector, a backscattered electron detector, a mirror for light collection, a dedicated aperture, a phase plate, an optical detector, and / or an X-ray detector. In another embodiment including one or more embodiments of the preceding embodiments, the functionalized sleeve includes one or more ports for a feedthrough of the stimulation component and / or the detection component to pass through. In another embodiment including one or more embodiments of the preceding embodiments, the axis is aligned with the length of the functionalized sleeve, and the one or more extensions protrude from the sample end of the functionalized sleeve along the axis of the functionalized sleeve. In another embodiment including one or more embodiments of the preceding embodiments, the functionalized sleeve includes a engagement mechanism at an end opposite to the sample end of the functionalized sleeve for engaging the functionalized sleeve with a charged particle microscope tube.

[0068] In one embodiment, a functionalized sleeve for a transmission electron microscope (TEM) sample holder includes: a cylindrical housing; one or more extensions extending from a first end of the cylindrical housing; a sensing and / or detection component coupled to the one or more extensions; and one or more ports in the cylindrical housing configured to allow a feedthrough of the sensing and / or detection component to pass through therethrough. In a first embodiment, an internal channel of the cylindrical housing is configured to receive the TEM sample holder, and when the sample holder is inserted into the cylindrical housing, the cylindrical housing circumferentially surrounds at least a portion of the length of the sample holder. In another embodiment, including one or more embodiments of the preceding embodiments, the one or more extensions extend above and / or below the sample end of the TEM sample holder in a direction along the length of the functionalized sleeve. In another embodiment, including one or more embodiments of the preceding embodiments, the one or more extensions include one or more holes aligned with the sample ring of the TEM sample holder, and the holes are aligned with the emission path of the electron beam when the TEM sample holder is inserted into the TEM barrel while being coupled to the functionalized sleeve. In another embodiment, including one or more embodiments of the preceding embodiments, the cylindrical housing includes one or more alignment fasteners along the outer and / or inner surfaces of the cylindrical housing. In another embodiment, including one or more embodiments of the preceding embodiments, the functionalized sleeve further includes a engagement mechanism at a second end of the cylindrical housing opposite to the first end, and the engagement mechanism includes one or more alignment posts for aligning the functionalized sleeve with the receiving port of the TEM barrel. In another embodiment, including one or more embodiments of the preceding embodiments, the one or more extensions include an inner portion of a vacuum transfer fitting surrounding the sample end of the TEM sample holder, and the functionalized sleeve further includes an outer portion of the vacuum transfer fitting configured to engage with a first end of the functionalized sleeve to isolate the sample end of the TEM sample holder from the surrounding environment around the functionalized sleeve.

[0069] In one embodiment, a method for using a sample support device including a functionalized sleeve includes: loading a sample onto a sample holder of the sample support device; positioning the sample in the path of a charged particle beam; activating a stimulation and / or detection component supported by the functionalized sleeve; and acquiring data from the sample when the sample is irradiated by the charged particle beam. In a first embodiment, the method further includes coupling an external portion of a vacuum transfer fitting to the sample end of the functionalized sleeve to hold the sample in a low-pressure environment within the vacuum transfer fitting. In another embodiment, including one or more embodiments of the preceding embodiments, when the sample support device is coupled to a charged particle microscope tube, the method further includes adjusting the vacuum transfer fitting from a closed position to an open position to position the sample in the path of the charged particle beam. In another embodiment, including one or more embodiments of the preceding embodiments, loading the sample includes positioning the sample near one or more extensions of the functionalized sleeve, and when the sample is loaded, aligning the sample with an aperture in each of the one or more extensions. In another embodiment, including one or more embodiments of the preceding embodiments, the sample holder is inserted into the functionalized sleeve such that the sample end of the sample holder protrudes beyond the sample end of the functionalized sleeve, and when the sample holder is inserted into the functionalized sleeve, the sample holder and the functionalized sleeve are coaxial along their lengths.

[0070] Although this disclosure has been described in detail with reference to specific embodiments, it will be apparent to those skilled in the art that various modifications and changes can be made without departing from the spirit and scope of this disclosure. Therefore, the specification and drawings are to be considered illustrative rather than restrictive.

Claims

1. A system comprising: A charged particle sample holder configured to hold a sample for analysis; and A functionalized sleeve configured to receive the charged particle sample holder into an opening extending along the axis of the functionalized sleeve, such that, when inserted, the functionalized sleeve encloses at least a portion of the charged particle sample holder. The functionalized sleeve includes one or more extensions arranged along the top or bottom of the sample, the one or more extensions including a stimulation component and / or a detection component.

2. The system of claim 1, wherein the functionalized sleeve further includes a vacuum transfer accessory capable of covering the sample end of the charged particle sample holder.

3. The system of claim 2, wherein the vacuum transfer accessory is adjustable between an open position and a closed position, and wherein in the open position the sample is exposed to the environment surrounding the charged particle sample holder, and in the closed position the sample is sealed within the vacuum transfer accessory.

4. The system of claim 1, wherein the stimulation component comprises one or more of a heating component, a cooling component, a gas supply portion directed toward the sample, a power source, a magnetic source, or a light source component.

5. The system of claim 1, wherein the detection component comprises one or more of a secondary electron detector, a backscattering electron detector, a mirror for light collection, a dedicated aperture, a phase plate, an optical detector, and / or an X-ray detector.

6. The system of claim 1, wherein the functionalized sleeve includes one or more ports for a feedthrough of the stimulation component and / or detection component to pass through.

7. The system of claim 1, wherein the axis is aligned with the length of the functionalized sleeve, and wherein one or more extensions protrude from the sample end of the functionalized sleeve along the axis of the functionalized sleeve.

8. The system of claim 1, wherein the functionalized sleeve includes a joining mechanism at an end opposite to the sample end of the functionalized sleeve for joining the functionalized sleeve to the charged particle mirror tube.

9. A functionalized sleeve for a sample holder in a transmission electron microscope (TEM), comprising: Cylindrical shell; One or more extensions extending from a first end of the cylindrical housing; Sensing and / or detecting components, said sensing and / or detecting components being coupled to said one or more extensions; and One or more ports in the cylindrical housing are configured to allow feedthroughs of the sensing and / or detection components to pass through them.

10. The functionalized sleeve of claim 9, wherein the internal channel of the cylindrical housing is configured to receive the TEM sample holder, and wherein when the sample holder is inserted into the cylindrical housing, the cylindrical housing circumferentially surrounds at least a portion of the length of the sample holder.

11. The functionalized sleeve of claim 9, wherein the one or more extensions extend above and / or below the sample end of the TEM sample holder in a direction along the length of the functionalized sleeve.

12. The functionalized sleeve of claim 9, wherein the one or more extensions include one or more holes aligned with the sample ring of the TEM sample holder, and wherein the holes are aligned with the emission path of the electron beam when the TEM sample holder is inserted into the TEM barrel while being coupled to the functionalized sleeve.

13. The functionalized sleeve of claim 9, wherein the cylindrical housing includes one or more alignment fasteners along the outer and / or inner surfaces of the cylindrical housing.

14. The functionalized sleeve of claim 9, wherein the functionalized sleeve further comprises a engagement mechanism at a second end of the cylindrical housing opposite to the first end, and wherein the engagement mechanism comprises one or more alignment posts for aligning the functionalized sleeve with the receiving port of the TEM tube.

15. The functionalized sleeve of claim 9, wherein the one or more extensions include an inner portion of a vacuum transfer fitting surrounding a sample end of the TEM sample holder, and wherein the functionalized sleeve further includes an outer portion of the vacuum transfer fitting configured to engage with a first end of the functionalized sleeve to isolate the sample end of the TEM sample holder from the surrounding environment around the functionalized sleeve.

16. A method for using a sample support device including a functionalized sleeve, the method comprising: Load the sample onto the sample holder of the sample support device; Position the sample within the path of the charged particle beam; Activate the stimulation and / or detection components supported by the functionalized sleeve; and Data is acquired from the sample when the sample is irradiated by the charged particle beam.

17. The method of claim 16, further comprising attaching an external portion of the vacuum transfer fitting to the sample end of the functionalized sleeve to maintain the sample in a low-pressure environment within the vacuum transfer fitting.

18. The method of claim 17, further comprising, when the sample support device is connected to the charged particle tube, adjusting the vacuum transfer accessory from a closed position to an open position to position the sample in the path of the charged particle beam.

19. The method of claim 16, wherein loading the sample includes positioning the sample near one or more extensions of the functionalized sleeve, and wherein when the sample is loaded, the sample is aligned with a hole in each of the one or more extensions.

20. The method of claim 16, wherein the sample holder is inserted into the functionalized sleeve such that the sample end of the sample holder protrudes beyond the sample end of the functionalized sleeve, and wherein when the sample holder is inserted into the functionalized sleeve, the sample holder and the functionalized sleeve are coaxial along their lengths.

Images