Heating assembly for charged particle beam system

Abstract

The invention relates to a heating assembly for a charged particle beam system. Systems, devices, and techniques for heating a sample are described. A heating assembly may include a film. The film may include a carbon nanotube material. The heating assembly includes a support that is mechanically coupled with the membrane. The support may be configured to be integrated with a charged particle beam system. The heating assembly also includes a heating circuit electrically coupled with the membrane. The heating circuit may be configured to direct current through the membrane.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to U.S. non-provisional application Ser. No. 18 / 595,124, filed Mar. 4, 2024, the disclosure of which is incorporated herein by reference in its entirety. Technical Field

[0003] Embodiments of the present disclosure relate to charged particle beam systems and components, algorithms, and methods for their operation. In particular, some embodiments relate to techniques for heating a sample. Background Art

[0004] In charged particle microscopy, characteristic x-rays are produced by exciting inner-shell electrons when the beam interacts with atoms in a sample. The x-ray signal is commonly used for elemental analysis in scanning electron microscope (SEM) systems. For example, the x-ray signal can be used to generate energy-dispersive x-ray (EDS) spectroscopy, which allows the elemental composition of a sample to be measured.

[0005] X-ray measurements are sensitive to EM radiation (e.g., infrared and visible photons), which can produce artifacts in EDS detector data. This presents a challenge when using EDS and other techniques sensitive to thermal photons to study the thermal properties of materials. Therefore, there is a need for improved sample heating systems that can be used with EDS detectors. Summary of the Invention

[0006] In a first aspect, a heating assembly includes a membrane. The membrane may include a carbon nanotube material. The heating assembly includes a support member mechanically coupled to the membrane. The support member can be configured to be integrated with a charged particle beam system. The heating assembly also includes a heating circuit electrically coupled to the membrane. The heating circuit can be configured to direct current through the membrane.

[0007] In some embodiments, the membrane defines a shape comprising a cone. The cone can be defined in a plane in Cartesian coordinate space. The shape comprises a biconical shape in the plane, such that the central region of the membrane is narrower than the peripheral region of the membrane. The heating assembly can be configured to be operably coupled to a sample stage of the charged particle beam system and used to position a sample on the heating assembly. The support member can include a conductive portion that is in electrical contact with the membrane and electrically coupled to the heating circuit. The heating circuit can be configured to direct the current through the membrane via the conductive portion. The support member can be shaped to be operably coupled to an electron microscope sample holder. The heating circuit can include a probe. The probe can be configured to be electrically coupled to the membrane or the support member. The probe can be a first probe, and the heating circuit can also include a second probe that is reversibly coupled to the membrane so that the current is directed from the first probe to the second probe via the membrane. The membrane can exist independently, at least partially, across an orifice defined in the support member. The carbon nanotube material can include a multi-walled carbon nanotube felt. The membrane can include multiple layers of carbon nanotube material. In some embodiments, the heating circuit includes a probe. The probe can be electrically coupled to the conductive portion of the support or the membrane. The probe can be mechanically coupled to the actuator and can be movable in one or more spatial dimensions. The probe can include a tip configured to interface with the membrane. The tip can include carbon nanotube material, can include filaments or other fibers resulting in a brush-like structure, and / or can be flexible.

[0008] In a second aspect, a charged particle beam system includes: a charged particle beam source; a sample chamber coupled to the charged particle beam source; and a heating assembly disposed within the sample chamber. The heating assembly may include, individually or in combination, one or more features described in the preceding aspects. For example, the heating assembly may include: a membrane comprising a carbon nanotube material; a support mechanically coupled to the membrane, the support reversibly coupled to a sample stage of the charged particle beam system, and configured to position a sample on the support and irradiate the sample with the charged particle beam generated by the charged particle beam source. The heating assembly may also include a heating circuit electrically coupled to the membrane and the charged particle beam system and configured to direct an electric current through the membrane. The heating circuit may be at least partially located outside the sample chamber. For example, one or more components of the heating circuit may be located outside the sample chamber and electrically coupled to one or more components within the sample chamber. In some embodiments, the system may also include an isolation chamber. The isolation chamber may include a fluid handling coupler and a deposition substrate. The deposition substrate may include a resistive heating circuit. The isolation chamber may define an orifice co-located with the deposition substrate. The isolation chamber may be disposed in the sample chamber. The orifice may be aligned with the charged particle beam source. The heating assembly may be at least partially disposed in the isolation chamber. The heating assembly may be disposed in the isolation chamber between the fluid handling coupler and the deposition substrate.

[0009] In a third aspect, a method for heating a sample comprises directing an electric current through a membrane of a heating assembly according to one or more of the preceding aspects. Directing the electric current through the membrane may comprise applying a power of about 30 W or less, about 20 W or less, about 10 W or less, about 5 W or less, about 4 W or less, about 3 W or less, about 2 W or less, about 1 W or less, about 0.5 W or less, about 0.4 W or less, about 0.3 W or less, about 0.2 W or less, and / or about 0.1 W or less, including fractions, subranges, or interpolated values ​​thereof, through the membrane.

[0010] In some embodiments, the membrane may have a sample disposed thereon. The method may further comprise removing material from the membrane in an area of ​​the membrane peripheral to the sample, and contacting the membrane with a probe electrically coupled to the heating circuit. The probe may contact the membrane in the area peripheral to the sample. Removing the material may comprise irradiating the membrane using a charged particle beam, using mechanical force, using directed EM radiation, and / or by igniting an arc or other discharge between the probe and the membrane.

[0011] The method may include heating the film to a temperature above the evaporation or sublimation temperature of the sample. The temperature may be determined at least in part based on the pressure in the isolation chamber and the composition of the sample. The method may include heating a deposition substrate. The deposition substrate may be heated to a substrate temperature below the evaporation or sublimation temperature of the sample. The method may include directing a charged particle beam and / or a photon beam toward the deposition substrate. The method may include exposing the deposition substrate to charged particles of the charged particle beam and generating deposition material on the deposition substrate. The charged particle beam may be directed using a scanning pattern. The deposition material may be disposed on the surface of the deposition substrate according to the scanning pattern. The method may also include introducing a carrier gas into the isolation chamber.

[0012] The terms and expressions that have been employed are used as terms of description and not of limitation, and in the use of such terms and expressions, there is no intention to exclude any equivalents of the features shown and described or portions thereof, but it is to be recognized that various modifications are possible within the scope of the claimed subject matter. It should be understood, therefore, that although the claimed subject matter has been specifically disclosed by way of embodiments and optional features, modifications and changes may be made to the concepts disclosed herein by those skilled in the art, and such modifications and changes are considered to be within the scope of the present disclosure as defined by the appended claims. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The foregoing aspects of the present disclosure and many of its attendant advantages will become more readily understood when the following detailed description is taken in conjunction with the accompanying drawings.

[0014] Figure 1A is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure.

[0015] Figure 1B is an example of a scanning electron microscope including various detectors according to some embodiments of the present disclosure. Figure 1A Schematic diagram of an example charged particle beam system's operation.

[0016] Figures 2A to 2H is a schematic diagram illustrating an example heating assembly according to some embodiments of the present disclosure.

[0017] Figure 3 is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure.

[0018] Figure 4 is a schematic diagram illustrating an example heating assembly according to some embodiments of the present disclosure.

[0019] Figure 5 is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure.

[0020] Figure 6 is a schematic flow chart illustrating an example method for localized heating of a material sample according to some embodiments of the present disclosure.

[0021] 7A to 7C is a schematic diagram illustrating an example configuration of one or more probes for heating of a material sample according to some embodiments of the present disclosure.

[0022] Figures 8A to 8B is an electron micrograph image showing heating of an example material sample according to some embodiments of the present disclosure.

[0023] Figures 9A to 9B is an electron micrograph image showing localized heating of an example material sample, according to some embodiments of the present disclosure.

[0024] FIG. 10A to FIG. 10B is an electron micrograph image showing localized heating of an example material sample, according to some embodiments of the present disclosure.

[0025] Figure 11 is a schematic diagram illustrating an example system for charged particle beam induced deposition according to some embodiments of the present disclosure.

[0026] In the accompanying drawings, unless otherwise indicated, like reference numerals refer to like parts throughout the various views. Where appropriate, not all instances of an element are labeled to reduce clutter in the drawings. The drawings are not necessarily drawn to scale, emphasis instead being placed on illustrating the principles being described. DETAILED DESCRIPTION

[0027] Although exemplary embodiments have been described, it should be understood that various changes may be made therein without departing from the spirit and scope of the present disclosure. The following paragraphs describe embodiments of analytical instrument systems, components, and methods for heating samples. To simplify the description, embodiments of the present disclosure focus on charged particle beam microscopy and microanalysis and related instruments. For this reason, the embodiments are not limited to such instruments, but are envisioned for analytical instrument systems, where the analysis of materials and temperature-dependent behavior may be complicated by the relative advantages of characteristic thermal radiation from heat sources near the sample. In an illustrative example, x-ray microanalysis may include generating detector data using a sensor that is sensitive to infrared photons emitted by the heating stage as noise that damages the quality of the x-ray signal. Such technology can benefit from improved heating component structures and configurations to reduce the infrared radiation flux reaching the detector. In addition, although embodiments of the present disclosure focus on electron beam systems, additional and / or alternative instruments and modalities are envisioned, including but not limited to ion beam systems or photon beam (e.g., laser) systems, etc.

[0028] Embodiments of the present disclosure include systems, methods, algorithms, and non-transitory media that store computer-readable instructions for heating a sample. In an illustrative example, a heating assembly may include: a membrane comprising a carbon nanotube material; a support mechanically coupled to the membrane, the support configured to be integrated with a charged particle beam system; and a heating circuit electrically coupled to the membrane and configured to direct an electrical current through the membrane. Advantageously, embodiments of the present disclosure reduce the thermal mass of the heating element, thereby reducing the flux of infrared radiation reaching a detector that can be attributed to the heating assembly, while also maintaining transparency to x-ray radiation, thereby filtering radiation leaving the sample to further reduce infrared artifacts in x-ray detector data. Additional advantages of the present disclosure include, but are not limited to, improved dynamic response, improved localization of heating to a single sample, compatibility with multiple samples, compatibility with multiple different charged particle beam systems, improved manufacturability relative to alternative heating sources (e.g., MEMS-based heating assemblies), and applicability for beam-induced deposition techniques (e.g., electron beam induced deposition (EBID) and / or ion beam induced deposition (IBID)).

[0029] Figure 1A is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure. The example charged particle microscope 100 includes multiple sections, including an electron source, a beam column 105, and a vacuum chamber 110. The electron source includes high voltage supply components, vacuum system components, and an electron emitter configured to generate an electron beam that is accelerated into the beam column 105. The beam column 105, in turn, includes an electromagnetic lens element configured to shape and form the electron beam from the electron source into a substantially circular beam having a substantially uniform profile transverse to the beam axis A, and to adjust the beam to be focused onto a sample 125 via an objective lens 115, as shown in reference Figure 1B Described in more detail.

[0030] Electron beams are typically characterized by the beam current and the accelerating voltage applied to produce the beam, among other criteria. The range of beam current and accelerating voltage can vary between instruments and is typically selected based on the material properties of the sample or the type of analysis being performed. However, typically, in scanning electron microscopes, electron beams are characterized by energies ranging from about 0.1 keV (e.g., for an accelerating voltage of 0.1 kV) to about 50 keV and beam currents ranging from picoamperes to microamperes.

[0031] The vacuum chamber 110 and / or the beam column 105 may include multiple detectors for various signals, including but not limited to secondary electrons generated by the interaction of the electron beam with the sample, x-ray photons (e.g., EDAX), other photons (e.g., visible light and / or IR cameras), and / or molecular species (e.g., TOF-SIMS), as described in reference Figure 1B The vacuum chamber 110 may also include a sample stage 120 that may be operably coupled to a multi-axis translation / rotation control system such that the sample 125 may be repositioned relative to the beam axis A as a means of investigating and / or imaging the sample 125. Figure 1A As described in more detail, the sample stage 120 may include a heating assembly 121, may be electrically coupled to the heating assembly, and / or may be mechanically coupled to the heating assembly. The heating assembly 121 may include a structure (e.g., a housing) that allows charged particles and / or other radiation (e.g., x-rays) to be transmitted through the sample and / or on which the sample is disposed. Figure 2B In this manner, one or more charged particle and / or radiation sensors of the present disclosure may be disposed in the vacuum chamber 110 and / or in the beam column 105 and configured to detect characteristic signals emitted (e.g., reflected and / or transmitted) from the sample, as described in reference to FIG. Figures 2A to 2H In this manner, heating assembly 121 can be configured to be operably coupled to sample stage 120, including electrical coupling (e.g., with a thermoelectric control system) and mechanical coupling (e.g., for translating and / or tilting the heating assembly using stage controls).

[0032] Example charged particle microscope 100 is illustrated as a single beam SEM instrument, in order to focus the description on the application of charged particle beam system in heating applications. In some embodiments, charged particle microscope 100 can be combined with an ion beam source (e.g., focused ion beam or FIB as a part of a dual beam system) suitable for, for example, modifying a sample or for microanalysis. Similarly, charged particle microscope 100 may include a photon source, such as a laser source or other electromagnetic radiation sources. In this way, the charged particle sensor of the present disclosure can be configured to coordinately generate detector data (e.g., image, line scan, x-ray spectrum, etc.) with the ion source for modification and / or microanalysis of the sample. In an illustrative example, a focused ion source (e.g., p-FIB, etc.) can be operably coupled with vacuum chamber 110 and is configured to incrementally remove the part of sample 125 in a layer-by-layer manner. Between increments, the x-ray microanalysis of sample 125 provides the depth distribution of the element information in sample 125, which is useful for the quality assurance in semiconductor applications and other fields.

[0033] Figure 1B is an example of a scanning electron microscope including various detectors according to some embodiments of the present disclosure. Figure 1ASchematic diagram of the operation of an example charged particle beam system. Detectors include a reflector detector (MD) 155, a pole piece mounted detector (PMD) 160, an EDS-adapted STEM mode detector (SMD) 165, and other detectors, such as a through the lens detector (TLD) 170 and an Everhart-Thornley detector 175. Other detectors and sources that may be coupled to the vacuum chamber 110 include a conventional x-ray detector 130 (e.g., a silicon drift detector configured for energy dispersive x-ray spectroscopy). Embodiments of the present disclosure include a charged particle microscope that includes an x-ray source, an x-ray detector, an ion beam source, a mass spectrometer, a light source (e.g., a laser source), or other sources that may be included in a supplement to an analytical instrument that may be used for SEM microanalysis. At least some of the detectors of the example microscope 100 may be paired with filters that are proximate to or covering an absorptive surface of the detector, as in reference to Figures 2A to 3 Described in more detail.

[0034] As illustrated, the mirror detector 155 and the TLD detector 170 are disposed in the beam column 105 or the objective 115. For example, the mirror detector 155 can be disposed above the objective 115 and oriented so that the sensor surface faces the sample stage 120. Advantageously, the positioning of the MD 155 in the beam column 105 makes the MD 155 well-suited for substantially flat samples 125 or for samples for which the sample stage 120 can be reoriented so that the normal angle is substantially aligned with the beam axis A, because in such cases the angular distribution of the emission from the BSE 180 is highest at a 45 degree angle to the surface of the sample 125. To focus on the position of the MD 155 relative to the BSE 180, the components of the microscope 100, and the sample 125, the following table describes the arrangement of the MD 155 relative to the BSE 180, the components of the microscope 100, and the sample 125: Figure 1B 155 is illustrated without a retaining member or other support structure. In some embodiments, the MD 155 is mounted on a retractable support 195, as illustrated by the SMD 165. In this manner, when the BSE 180 imaging / analysis mode is activated by a user of the charged-particle microscope 100 and subsequently retracted from a position in the beam column 105 and / or objective 115, the MD 155 can be introduced into that position. In some embodiments, the MD 155 is mechanically coupled to components of the beam column 105 and / or objective 115 and remains in place when not in use.

[0035] The pole piece mounted detector 160 may be mechanically coupled to the pole piece 117 housing the objective lens 115 and oriented so that the collector surface faces the sample stage 120. As with the MD 155, the PMD 160 may be mounted on a retractable support 195 rather than being mechanically coupled to the pole piece 117. Advantageously, mounting the PMD 160 on the retractable support 195 allows the PMD 160 to be removed from between the sample stage 120 and the pole piece 117, thereby allowing other probes, sources, or components to be introduced into the space (e.g., a parabolic reflector for luminescence measurement and / or imaging).

[0036] An adapted STEM mode detector 165 (configured as an energy dispersive spectrometer (EDS) detector) can be mechanically coupled to a retractable support 195 that is configured to introduce the SMD 165 into a position such that the sample stage 120 is located between the objective lens 115 / pole piece 117 and the SMD 165. The SMD 165 can be oriented so that the detector surface faces the underside of the sample stage 120. In this manner, x-rays 181 emitted from the sample 125 (e.g., a region of the sample's interaction volume where x-rays are generated) can reach the detector surface and generate characteristic signals for imaging and / or microanalysis. The x-rays 181 can include x-rays generated from inner shell excitations in atoms of the sample 125 that are directed through the sample rather than back toward the beam column 105. Forward scattered electrons (FSEs) emitted from the sample 125 can be absorbed by the heater element membrane, which is characterized by relatively low electron transmittance, before reaching the detector surface, producing artifacts (e.g., background signals) in the data. In some embodiments, the membrane can be thin enough to allow some transmission of FSEs, thereby allowing STEM mode imaging and / or microanalysis of the sample. For a given FSE energy range, the thickness of the membrane can be determined at least in part based on the transmittance of the membrane material as a function of thickness.

[0037] The x-ray detector 130 includes a detector 131 that is shielded from charged particles, photons, and other noise sources by a window 133 and a collimator 135, the overall result of which is a significant reduction in the solid collection angle. Additionally, to protect the window material and / or reduce interaction between magnetic components of the x-ray detector 130 and the charged particle beam, the x-ray detector 130 may be limited to a relatively low take-off angle, e.g., about 30 degrees to about 50 degrees measured from a plane defined by the sample 125. The take-off angle may be increased by tilting the sample 125, at the expense of reduced functionality of the detectors 155, 160, 165, and 170 during x-ray collection.

[0038] Figure 2Ais a schematic diagram illustrating an example heating assembly 200 according to some embodiments of the present disclosure. The heating assembly 200 includes a membrane 210 in a support 215. The support 215 includes one or more contact portions 220. The contact portions 220 can operably couple (e.g., thermally couple, mechanically couple, etc.) the membrane 210 and / or the support 215 to one or more coupling members 225, through which the heating assembly 200 can be coupled to a sample stage (e.g., Figure 1A to Figure 1B The membrane 210 comprises a plurality of layers 211 of filter material, as shown in FIG. Figure 2B Detailed description. The support member 215 may be coupled to the membrane 210 over at least a portion of the periphery of the membrane 210. In this manner, the support member 215 mechanically supports the membrane 210, thereby allowing the membrane 210 to at least partially exist independently over the area of ​​the heating assembly 200. In the illustrated example, the support member 215 forms a frame over which the membrane 210 extends, allowing the membrane 210 to exist independently over the orifice defined by the frame. Advantageously, the sample is disposed over the area of ​​the heating assembly 200 so that the sample is supported by the membrane 210, allowing the sample to be heated by the membrane and irradiated by the charged particle beam to produce a detectable characteristic signal.

[0039] Embodiments of the present disclosure can be configured to be operably coupled to a charged particle beam instrument. For example, the coupling member 225 can include an electrical coupler, a mechanical coupler, an optical coupler, or the like to facilitate integration of the heating assembly 200 with the sample stage of the charged particle beam system. In the example of an SEM system, the coupling member 225 can include: two electrical contacts configured to electrically couple to elements of a heating circuit; and one or more mechanical couplings (e.g., a clamp, a tab-slot coupling, etc.) to mechanically hold the heating assembly in place when coupled to the sample stage. In this way, the heating assembly 200 can be moved using the stage controls of the SEM system and current can be directed through the membrane 210.

[0040] Film 210 may include a material that exhibits selective transmittance for x-rays 275. Selective transmittance refers to the ability of film 210 to allow at least a portion of incident x-rays 275 of a given energy to pass through the film 210 while absorbing relatively low-energy photons (e.g., UV-visible-IR photons) below a given threshold energy and absorbing or reflecting at least a portion of electrons incident on the film 210. For example, film 210 may absorb, reflect, or otherwise block substantially all electrons with energies of approximately 7.8 keV or less. In some embodiments, the threshold energy may be selected based at least in part on the thickness of the filter and / or the density of the filter as parameters. For example, a filter having a thickness of approximately 2 μm may block incident electrons with energies below approximately 2.5 keV. Below 7.8 keV, the thickness dependence of the filter performance allows for adjustment of operating conditions. Furthermore, the threshold energy may depend at least in part on the composition of film 210. For example, a film 210 comprising multi-walled carbon nanotubes may be characterized by a higher threshold energy relative to a film 210 comprising single-walled carbon nanotubes, based at least in part on the mass density of the film 211. Similarly, a film 210 having a relatively high density of nanotubes per unit surface area may be characterized by a higher threshold energy than a film 210 having a relatively low density of nanotubes per unit surface area.

[0041] In exemplary embodiments, areal density is defined as the mass of membrane 210 material per unit surface area (e.g., square centimeters). The properties of membrane 210 can be described and / or related via areal density based, at least in part, on characteristic volumetric properties, including the bulk density of the carbon material (e.g., mass / volume) and / or the void fraction of the membrane (e.g., the average proportion of void space in the membrane). In some embodiments, the bulk density of the carbon material is about 0.11 g / cm 3 to about 1.1 g / cm 3 , including subranges, fractions, and interpolated values ​​thereof. In some embodiments, transparency and thickness are inversely related. For example, for a given areal density, a film thickness of about 1.32 μm may correspond to a transmittance of about 3.5% at 550 nm, while a film thickness of about 2.64 μm may correspond to a transmittance of about 0.12%. In this way, for a given film, both the thickness and transparency of the film may be referenced to the areal density. For example, the areal density may be about 0.1 μg / cm 2 to about 330mg / cm 2 , including subranges, fractions, and interpolated values ​​thereof, thereby allowing the size, number of layers, and individual layer thickness of film 210 to be determined based at least in part on a balance between transparency and size / space constraints.

[0042] In some embodiments, the membrane 210 includes a carbonaceous material 213. The carbonaceous material 213 may include a carbon nanotube material. The carbon nanotube material may include single-walled nanotubes, double-walled nanotubes, multi-walled nanotubes, and / or mixtures thereof. The carbonaceous material 213 may include carbon nanofibers, nanofibers, other forms of sp 2 Hybridized carbon, sp 3 Hybridized carbon and / or their mixtures (e.g., a combination of graphite and amorphous carbon). Nanotubes, nanotubes and / or nanofibers may be oriented along one or more in-plane directions and / or may be randomly oriented. For example, film 210 may include layers in which the carbon nanotubes constituting the carbon nanotube felt are substantially aligned with the orientation direction. Different layers may be oriented in the same direction or in different directions. Although substantially aligned with the orientation direction over a given layer and / or film 210, individual nanotubes, nanofibers, etc. may exhibit tortuosity (e.g., bending, angled / kinked, looped and / or spirally twisted segments) such that segments of a given nanotube, nanofiber, etc. may be oriented away from the orientation direction. Film 210 may also include metal, ceramic and / or nitride materials, for example, as coatings, inclusions, or other forms that substantially do not limit the transmittance and / or thermal properties of film 210.

[0043] The film 210 may have a thickness on the order of about 10 nm to about 10 μm (e.g., about 10 nm to about 99 μm), including subranges thereof (e.g., about 0.5 μm to about 30 μm), fractions thereof, and interpolated values. The film 210 may include multiple layers 211 of carbon nanotube material ranging from about 3 nm thick to about 1 μm thick, individually including subranges thereof, fractions thereof, and interpolated values. In an example, each layer may have a thickness of about 0.4 μm, such that a film having two layers of carbon nanotube material may be about 0.8 μm thick, and a film having 25 layers of carbon nanotube material may be about 10 μm thick. Without being limited to a particular physical phenomenon or mechanism, the filter 210 may have a thickness-dependent transmittance based at least in part on the absorbance of each constituent layer. In this manner, the film 210 may include multiple layers that allow the filter 210 to absorb substantially all incident photons and / or charged particles while allowing transmission of a significant portion of the x-rays 275.

[0044] Each layer can have a photon absorptivity of about 1% to about 90% (e.g., as measured at 525 nm). In the example of 25 layers of carbon nanotube material, each of which has an absorptivity of about 40% at 525 nm, the total absorption factor of film 210 for photons at 525 nm can be about 1×10 -9In the example of a film 210 having a thickness of about 2 μm, the transmittance of LiKα (55 eV) x-rays 275 can be about 23%, corresponding to a significant improvement over current bulk heating stages that are opaque to x-rays. In addition, comparative example detectors of the prior art that include carbon materials as part of the window layer typically include support grids that introduce artifacts and opaque aluminum coatings on at least one surface of the window layer, which further reduces the quantum efficiency of the detector. In contrast, the films of the present disclosure may include a frame (e.g., Figure 2A The at least partially unsupported membrane 210 is maintained by a support member 215) surrounding at least a portion of the membrane 210.

[0045] Figure 2B The membrane 210 is illustrated as being electrically coupled to the electronic components of the heating circuit 230 via the contact portion 220. For example, the membrane 210 may make electrical contact with the contact portion 220. The electronic components may include one or more power supplies 235. The heating circuit 230 may be located at least partially within the sample chamber (e.g., Figure 1A to Figure 1B For example, one or more components of the heating circuit may be located outside the sample chamber and electrically coupled (eg, via electrical feedthroughs) to one or more components inside the sample chamber.

[0046] In this manner, an electric potential (e.g., a voltage) can be applied across the membrane, thereby directing current through the membrane and inducing resistive heating. Advantageously, utilizing or forming membrane 210 from a carbon nanotube material can improve the performance of heating assembly 200 as a heating stage while retaining the performance of the heating assembly for retaining and / or detecting a characteristic signal from a sample disposed on membrane 210.

[0047] In this context, the performance of the heating assembly 200 as a heating stage for sample microanalysis refers, at least in part, to one or more properties of the membrane 210 as the resistive heating element 240. For example, the resistive heating element 240 can be characterized by dynamic properties (e.g., rise time) and material properties (e.g., thermal mass). The conductive carbon nanotube material is characterized by improved thermal radiation properties relative to comparable resistive heating materials (such as carbon fiber materials or tungsten-based materials, etc.), which allows the example heating assembly 200 to generate relatively less thermal radiation (e.g., infrared and visible photons) than other materials at comparable temperatures and reach the set point temperature in a relatively shorter time. Advantageously, the relatively low thermal radiation allows the heating assembly of the present disclosure to be smaller than conventional integral heating stages, in which the membrane 210 (rather than the integral material) is exposed to an elevated temperature. This, in turn, reduces the thermal mass being heated and allows heating rates of up to approximately 10,000 Kelvin per second. This represents a significant improvement in heating rates relative to conventional integral heating stages.

[0048] Figures 2C to 2HSchematic diagrams illustrating multiple example configurations of the membrane 210 of the example heating assembly 200 according to some embodiments of the present disclosure. The shape of the membrane 210 in one or more spatial dimensions can affect the behavior and performance of the membrane 210 as a heating element. Without being constrained by a specific physical mechanism, the power dissipated in the membrane 210 can be a function of the current directed through the membrane 210 and the voltage drop across the membrane 210. The heat generation at a given location in the membrane 210 is a flux quantity, so that the local temperature of the membrane 210 can be related to the power dissipated in the membrane 210 and the geometric cross-section of the membrane at a given location. In this way, the temperature can be a local property for a given current, where the narrower portion of the membrane 210 is hotter than the wider portion of the membrane 210.

[0049] to this end, Figure 2C An example film 210 is illustrated defining a shape including a cone 245. The cone may be defined in a plane in a Cartesian coordinate space. Figure 2C In the example of FIG. 2 , the taper 245 is defined in the XY Cartesian plane so that the width of the membrane 210 in the "Y" dimension can be expressed as a function of the position in the "X" dimension. The letters "X" and "Y" are used for convenience and do not refer to true horizontal or vertical directions. The shape can include multiple taper angles, examples of which are shown in FIG. Figure 2C As shown in FIG, the shape includes multiple sides ranging from 3 to 20 sides or more. For example, a four-sided pyramidal membrane may define a trapezoidal shape, while Figure 2C A bi-conical shape in this plane is illustrated such that a central region 250 of the membrane 210 is narrower than a peripheral region 255 of the membrane 210 .

[0050] In some embodiments, the membrane 210 defines a shape that includes a cone defined in multiple planes. The shape may include cones in the XY plane and the XZ plane in Cartesian space. Figure 2D In the illustrated example embodiment, the shape of the membrane 210 includes a three-dimensional taper from a first cross-sectional area in the YZ plane near the support portion 220 to a relatively smaller second cross-sectional area in the YZ plane near the central region of the membrane 210. Figure 2CAs with the conical shape described above, the electron flux passing through the membrane can heat the central region 250 to a relatively higher temperature than the peripheral region 255. As described in more detail with reference to Examples 1 to 3, the membrane 210 can be repeatedly heated to a temperature at which the sample 260 disposed on the membrane 210 can undergo a phase transition. In this context, the term "phase transition" can refer to a change from a solid phase to a liquid phase (e.g., melting), but can also refer to other types of phase transitions, such as a crystalline phase structure that depends on temperature and / or pressure. In an illustrative example, a crystalline sample can be heated to induce a transition from a first crystalline phase to a second crystalline phase, and the transitions between the phases can be imaged using a SEM (e.g., BSE channeling contrast) / using a FIB or using electron microscopy analysis techniques (e.g., electron beam diffraction, x-ray spectroscopy, etc.). Advantageously, the heating assembly of the present disclosure allows for interrogation of one or more physical phases and / or phase transitions under charged particle irradiation. The membrane 210 exhibits improved heating properties and significant transparency to characteristic signals generated by the interaction of the sample 260 and the beam of charged particles 190.

[0051] Figures 2E to 2H An alternative example embodiment is illustrated that includes an orifice 265 formed in the membrane 210, through which an electrical current can be directed through the membrane 210 in a manner that produces a relatively high temperature in a localized area of ​​the membrane 210. Advantageously, defining one or more orifices 265 in the membrane 210 can improve the structural stability of the membrane while imparting improved heating behavior (e.g., by reducing the effective cross-section of the membrane 210). In addition, defining the cross-section as a function of position in the membrane 210 by patterning the orifices 265 in the membrane 210 can improve manufacturability and / or can allow the membrane 210 to be prepared in situ in the presence of the sample 260. In the illustrative examples, a beam of charged particles (e.g., ions, electrons, etc.) and / or a beam of photons (e.g., laser) can be directed toward the membrane 210 and used to pattern the orifices 265, as described in reference to Figure 6 Described in more detail.

[0052] Figure 3 is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure. In the following description, for simplicity, details of the internal components and functions of the example TEM system 300 are omitted, and the description is focused on the embodiments of the present disclosure, as shown in FIG. Figure 4 An example TEM system 300 includes an electron source section, a TEM column including a sample section 305, and an imaging section 310. The present disclosure focuses on techniques for improving the performance of heating assemblies used in the sample section 305.

[0053] Briefly, the electron source section includes electronic devices configured to excite a charged particle source, which may include a high voltage field emission source or other emitting electron source, so that an electron beam is formed and conducted through a vacuum into the TEM column. The TEM column includes components for beam forming, including electromagnetic lenses and / or electrostatic lenses and a plurality of apertures to control the properties of the electron beam. The TEM column components include a condenser lens, an objective lens, a projection lens, an aberration corrector, a deflector, an stigmator, etc. and corresponding apertures. The sample section 305 accommodates the sample 260 (refer to FIG. 2 ) disposed on the heating assembly. Figure 2A ), the electron beam can pass through the heating element, as shown in the reference Figure 4 Described in more detail, the sample section may include one or more types of detectors, such as x-ray detectors, secondary electron detectors, and the like.

[0054] The most advanced TEM column may have up to four condenser lenses for flexible (e.g., stepwise or graded) demagnification and focusing of the electron beam on the sample, and up to five projection lenses for flexible magnification of the electron beam downstream of the sample to the detector, as well as up to two aberration correctors. Since the most advanced aberration correctors may include additional lenses and several multipoles (e.g., four lenses and two to three or more multipoles), a modern TEM column may include up to about twenty lenses. The coordinated operation of the overall lenses and other optical elements results in a given demagnification at the sample and a given magnification at the detector.

[0055] The detector section 310 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 imaging section may include a scintillator screen, binoculars, a transmission electron microscopy (TEM) detector (e.g., a pixelated electron detector, a secondary electron detector, a camera), a segmented STEM detector, and an electron energy loss spectroscopy (EELS) spectrometer 315, among others. The EELS spectrometer 315 acts at least in part as an energy filter by focusing the electron beam onto an electrostatic or magnetic dispersive element (also known as a "prism"), which exerts a force on the electrons that is proportional to their velocity. In this way, electrons that have transferred energy to the sample (e.g., via inelastic collisions) can be redirected through the magnetic dispersive element and toward the detector. The detector may include a pixelated detector (e.g., a CCD device configured to detect electrons) that generates one-dimensional or two-dimensional EELS data, from which an EELS spectrum can be derived. In some embodiments, the EELS spectrometer 315 further includes one or more optical elements, such as electromagnetic or electrostatic lenses and / or multipoles and / or accelerators, to condition and / or focus the scattered electrons onto a detector.

[0056] Figure 4 is a schematic diagram illustrating an example heating assembly 400 according to some embodiments of the present disclosure. Figures 2A to 2H The embodiment of the example heating assembly 200 is described, wherein the heating assembly 400 is configured to be operatively coupled to a TEM sample holder 405. To this end, the example heating assembly 400 includes one or more membranes 410 and one or more frames 415, the one or more frames including one or more conductive portions 420. The conductive portions 420 can be coupled to components of a heating circuit (e.g., as described in reference Figure 2B The heating circuit is configured to electrically couple the frame 415 to the sample holder 405 and / or the TEM system (e.g., Figure 3 In the illustrative example, electrical coupling of the frame 415 to the heating circuit can be facilitated by forming one or more conductive contacts 430 on the frame 415 and using one or more conductive probes 435.

[0057] The frame 415 can be or include a TEM grid or a component of a TEM grid, such that a conventional TEM grid holder can be adapted for use with the heating assembly 400. Where conventional heating holders include electrical contacts, traces, etc., such that the sample placement position is relatively restricted relative to the heating position, the film 410 of the present disclosure can allow for relatively unrestricted sample placement facilitated by probe positioning when the probe is electrically coupled to the film 410, as described with reference to FIG. Figures 6 to 7C Described in more detail. In this manner, the heating assembly of the present disclosure allows samples 460 to be heated individually.

[0058] Advantageously, integration of the heating assembly of the present disclosure into a TEM / STEM instrument can enable detector data to be generated at spatial resolution levels exceeding those available in SEM instruments. Furthermore, TEM / STEM analysis enables crystal structure analysis of nanostructured sample 460 and enables the probing of temperature-dependent properties of sample 460 at the nanoscale. To this end, embodiments of the present disclosure include a film 410 that is substantially transparent to electrons (e.g., above a given threshold energy) and substantially transparent to x-rays (e.g., outside one or more characteristic energies associated with the film material).

[0059] Figure 5 is a schematic diagram illustrating an example charged particle beam system according to some embodiments of the present disclosure. The example system 500 includes instruments 505 (e.g., Figure 1A to Figure 1B The example system 100 includes an instrument computing device (IPC) 510 and a client computing device 515. The example system 500 includes a heating circuit (e.g., as shown in FIG. Figures 2A to 2HThe apparatus 505 includes a probe assembly 530 electrically coupled to components of the heating assembly 525 (described above). The apparatus 505 includes a test section 545 in which the probe assembly 530 is disposed, including a vacuum component for isolating the heating assembly 525 from the atmosphere. Coupled to the test section are a charged particle column 540 and one or more detectors 550. The charged particle column 540 can be an ion beam (e.g., a focused ion beam (FIB)) column or an electron beam column. In some embodiments, the apparatus 505 includes a FIB column and an electron beam column, wherein one of the charged particle sources is coupled to the vacuum chamber at an angle relative to the charged particle column.

[0060] The electron beam column can generate an electron beam 547 and focus the electron beam 547 onto the heating assembly 525. The interaction of the electron beam 547 with the heating assembly 525 generates one or more detectable signals that can be received by one or more detectors 550 operatively coupled to the vacuum chamber 545 and configured to generate detector data based at least in part on measurements of the signals. In the illustrative examples, the detectors 550 can include secondary electron detectors, backscattered electron detectors, photon detectors, imaging sensors (e.g., CCDs), or x-ray detectors, among others.

[0061] Compared to a typical scanning electron microscope (SEM), the vacuum chamber 545 can omit sample manipulation tools (such as interlocks and sample stages), at least in part because the heating assembly 525 can be removably coupled to a probe assembly 530, which can be disposed on a stage, bracket, or other holding assembly that provides electrical and thermal coupling to the test section. The electron beam 547 can be directed toward the heating assembly 525 using various operating modes, including but not limited to imaging mode, line scan mode, and / or fixed-point mode. The probe assembly 530 can include individually addressable probes 555 that can be moved in three spatial dimensions (labeled by the "xyz" Cartesian axes) via an electromechanical actuator 560. In this manner, the probe tip can be displaced toward a location on the surface of the heating assembly 525 with nanometer-level precision. In some embodiments, the probe assembly 530 is electrically coupled to components of the test section 535 via couplings 565 and 570, thereby driving the actuator 560 (e.g., using a drive signal) and generating an output signal.

[0062] The computing devices 510 and 515 can be general-purpose machines (e.g., laptop computers, tablet computers, smart phones, servers, etc.) configured to operate the instrument 505 or otherwise interact with it. The instrument 505, in turn, can include electronic components that form part of a dedicated computing device, including control circuits configured to drive the test circuit, actuate the probe assembly 530, control the electron beam column 540, and operate the vacuum system and thermal management system. The IPC 510 can be a machine provided with software that is configured to interface with the instrument 505 and allow a user of the instrument 505 to perform tests on the heating assembly 525. Similarly, the client PC 515 can be configured to control one or more systems of the instrument 505 (e.g., via the IPC 510 and / or by interfacing with the instrument 505 via the network 520) to perform tests on the heating assembly 525. In some embodiments, the instrument 505, IPC 510, and / or client PC 515 are in separate physical locations and are coupled via a network 520 and / or by other means, such as a direct connection or by a wireless connection (e.g., near-field radio). The network 520 may include a public network (e.g., the Internet) and / or a private network (e.g., an intranet or a local area network). In some embodiments, the IPC 510 and / or client PC 515 are configured to operate the instrument autonomously (e.g., without human intervention) or semi-autonomously (e.g., with limited human intervention, such as initiating a test, identifying a sample, and / or confirming automated analysis results).

[0063] Figure 6 is a schematic flow chart illustrating an example process for localized or partially localized heating of a material sample according to some embodiments of the present disclosure. One or more operations of the example process 600 may be performed by a computer system in communication with additional systems, including but not limited to instrumentation systems, network infrastructure, databases, and user interface devices. In some embodiments, reference Figure 6 At least one subset of the operations described is performed automatically (e.g., without human involvement) or pseudo-automatically (e.g., initiated by a human or with limited human intervention). In the illustrative examples, operations for positioning the probe tip, displacing the probe tip, generating and / or directing a charged particle beam, isolating a sample, and directing current through a heating assembly may be performed automatically or pseudo-automatically. Although the example process 600 is described as a sequence of operations, it should be understood that at least some of these operations may be omitted, repeated, and / or reordered. In some embodiments, additional operations are performed before and / or after the operations of the example process 600, which are omitted for clarity of explanation, such as operations for electron source calibration, alignment and aberration correction of the electron beam, or initialization of probe positioning. In this context, "local" and "partially local" refer to the use of one or more movable electrical contacts (e.g., Figure 5The probe 555) directs the current to a membrane close to the sample (e.g., Figure 2A In this way, the current can be directed from the movable electrical contact to the conductive portion of the heating element (e.g., Figure 2A conductive portion 220) and / or guided from one movable contact to another movable contact.

[0064] At operation 605, the example process 600 includes identifying a sample. Identifying a sample may include locating a sample (eg, Figures 2A to 2H Identifying a sample 260) may include one or more sub-operations. Identifying a sample may include image processing sub-operations, which may include manual intervention, automatic edge finding, and / or feature tracking algorithms by which the film may be localized on the film. In this context, an image may include various detector data (e.g., secondary electron image data, backscattered electron image data, light camera image data, etc.) generated by a charged particle beam system.

[0065] At operation 610, the example process 600 includes directing charged particles toward the membrane 210. In the context of operation 610, the charged particles may include electrons and / or ions. In some embodiments, the current of charged particles may degrade or otherwise remove material of the membrane 210 in a specified location on the membrane 210. To this end, a charged particle beam (e.g., generated using an SEM or other charged particle beam system) and / or by biasing the probe 555 relative to the membrane (or vice versa) and inducing a current between the probe 555 and the membrane 210 can be used to direct the charged particle stream toward the membrane.

[0066] At operation 615 , the example process 600 includes forming one or more apertures 640 (eg, Figures 2E to 2H 1 , removing material from the membrane 210 to at least partially isolate the sample 260 on a portion of the membrane 210. Isolating the sample 260 may include: Figure 5 The film 210 can be patterned by scanning control signals (associated with scanning circuitry of the example system 500, etc.) such that charged particles are incident on the film 210 at multiple locations along the path 635. For example, the probe 555 can be biased relative to the film such that current can be used to locally ablate the film (e.g., by igniting an arc, pulsing an arc, etc.) and form the orifice 640.

[0067] To this end, operations 610 and 615 of the example process 600 may be parallelized and / or serialized in multiple iterations. For example, a charged particle beam (e.g., Figure 5The beam 547 of the primary electrons is directed so that the current of the primary electrons can be used to form the aperture 640. In this manner, a region 645 of the film 210 peripheral to the sample 260 can be at least partially isolated and used for localized electrical heating of the film 210 and the sample 260. In some embodiments, operation 615 can also include mechanically engraving the aperture 640 using the probe 555 and / or ablating the film material using an EM radiation source (e.g., a laser, a pulsed laser, etc.).

[0068] At operation 620, the example process 600 includes positioning the probe 555 to form electrical contact with the membrane 210 within the peripheral area 645 defined by the orifice 640. Although the probe 555 is illustrated as having a defined conical shape, embodiments of the present disclosure include probes 555 having additional or alternative geometries. For example, the probe tip may define an irregular, branched, brush-like, or otherwise configured shape to reduce the likelihood that the probe 555 will pierce the membrane 210 rather than forming a durable electrical contact. In some embodiments, the probe 555 includes surface roughness and relatively high flexibility as a means of improving the quality of contact with the membrane 210.

[0069] At operation 625, the example process 600 includes directing current through the membrane 210, using the probe 555 to localize the current through the peripheral region 645. In this manner, the region 645 is heated to a relatively high temperature compared to the membrane material outside of the region 645. In the case where a single probe 555 is used to direct current through the membrane 210, the probe 555 may be coupled to a heating assembly (e.g., Figure 2A Example heating assembly 200, Figure 4 Example heating assembly 400, Figure 5 The conductive portion of the support element (e.g., the example heating assembly 525, etc.) Figure 2A The current is conducted between one or more conductive parts in the portion 220). 7A to 7C As described in greater detail, the number and relative positions of probe tips 555 and orifices 640 may vary.

[0070] Advantageously, the example process 600 allows for localized heating of a single sample 260 on a membrane 210 that may otherwise support one or more other samples, such as Figure 4 To this end, a single sample preparation and loading process can be used to prepare multiple replicate microanalytical experiments, thereby increasing throughput and efficiency in terms of time and complexity of preliminary operations.

[0071] 7A to 7C is a schematic diagram illustrating an example configuration of one or more probes for heating a material sample according to some embodiments of the present disclosure. An example embodiment of a multi-probe configuration and a membrane including a plurality of orifices 640 is illustrated. Figure 7AIn the two probes (e.g., Figure 5 The probe 555 is electrically coupled to the membrane 210 near the sample 260 and serves to limit the portion of the membrane 210 through which the current is directed. In this manner, the present disclosure may be performed in an exemplary process (e.g., Figure 6 Omit operations for removing membrane material from at least some iterations of the example process 600). Figure 7B In, reference Figures 2C to 2H The described techniques may be adapted to define a peripheral region 645 near a sample in which the pattern defined as part of the example process 600 (e.g., Figure 6 610 and 615) may include a plurality of apertures 640 that together separate the sample and peripheral region 645 from the heating assembly support structure (e.g., Figure 2A Support member 215, Figure 2A One or more of the conductive portions of the conductive portion 220, etc.) are at least partially isolated. Figure 7C In the embodiment of the present invention, multiple probes 555 electrically coupled to the membrane 210 are used to define multiple conductive paths. A plurality of orifices 640 are used to define the peripheral region of the membrane. Advantageously, the illustrated multi-path configuration allows for subtle dynamic and spatially localized heating of the sample, for example, when the membrane 210 and / or the sample exhibit anisotropic conductivity / resistivity or other thermal and / or electrical properties. For example, a four-probe configuration allows for resistance measurements of the region defined by the orifices 640, from which the membrane temperature can be estimated.

[0072] Example 1: Local heating of various material samples

[0073] The following paragraphs describe experimental data generated using the system of the present disclosure. The images below represent detector data that reveal the phase transition from solid to liquid of various metal particles disposed on a film through which an electric current was directed to induce heating. The data indicate that, at least near the sample, the film was heated to the point where the metal melted and became liquid or amorphous. The experimental conditions included a film of multi-walled carbon nanotubes and a direct current (e.g., a DC current) of about 3 watts to about 5 watts for non-local heating to about 1350 K. Figures 2A to 2H and a direct current of about 0.2 W to about 0.6 W for local or partial local heating to a comparable temperature (e.g., Figures 6 to 7C The experiment duration was about 30 seconds, and the film heating time was significantly shorter, heating from about 300 K to about 1300 K in about 0.1 seconds.

[0074] Figures 8A to 8Bis an electron micrograph image showing heating of an example material sample according to some embodiments of the present disclosure. The sample comprises gold, which is characterized by a melting temperature of 1337 K under SEM conditions. In this manner, the membrane is capable of reversibly heating the sample to a temperature of 1337 K or above using electrical heating induced by passing an electric current through the membrane.

[0075] Figures 9A to 9B is an electron micrograph image showing localized heating of an example material sample according to some embodiments of the present disclosure. The sample comprises silicon, characterized by a melting temperature of 1687 K under SEM conditions. In this manner, the membrane is capable of reversibly heating the sample to a temperature of 1687 K or above using electrical heating induced by directing an electric current through the membrane. Figures 9A to 9B The experiments on the data in the Figure 6 At least some of the operations of the example process 600 are performed, whereby a peripheral region of the membrane is confined near the sample and the probe tip is used to direct a heating current through the membrane. The formation of a smooth surface and the aggregation of the sample material into a spherical shape reveal a phase transition of the silicon, consistent with the physical tendency to minimize surface energy in liquids.

[0076] FIG. 10A to FIG. 10B is an electron micrograph image showing localized heating of an example material sample according to some embodiments of the present disclosure. The sample comprises platinum, characterized by a melting temperature of 2041 K under SEM conditions. In this manner, the membrane is capable of reversibly heating the sample to a temperature of 2041 K or above using electrical heating induced by directing an electric current through the membrane. Figures 9A to 9B The experiments on the data in the Figure 6 At least some of the operations of the example process 600 are performed whereby a peripheral region of the membrane is defined adjacent the sample and the probe tip is used to direct a heating current through the membrane. Figure 10B The deformation of the film observed in is attributed to the surface tension effects of platinum in forming droplets (eg, minimizing surface energy) while maintaining wetting of the film surface.

[0077] Example 2: Generating Precursor Vapors for EBID / IBID Processes

[0078] Figure 111 is a schematic diagram illustrating an example system 1100 for charged particle beam induced deposition according to some embodiments of the present disclosure. Example system 1100 includes an isolated chamber 1110 for containing vapor generated by heating a sample material 1120 using a heating assembly 1125 of the present disclosure. A carrier gas can be introduced via a conduit 1115 fluidically coupled to the chamber. The carrier gas can entrain the evaporated sample and conduct the vapor to the vicinity of a deposition substrate 1130. A charged particle beam 1135 (e.g., an ion beam, an electron beam, etc.) and / or a photon (e.g., a laser) beam can be directed toward the deposition substrate 1130 to induce a deposition process, wherein the vapor serves as a deposition precursor. Such techniques can be used to deposit patterns of material 1140. The deposited material 1140 can be chemically identical, similar, or different from the sample material from which the precursor was generated. For example, a variety of precursors can be generated using one or more heating assemblies of the present disclosure, such that the beam-induced deposition process includes a chemical reaction of the precursors that produces the solid deposition material. In some cases, the deposition process uses the energy of the beam (e.g., when using inert ions such as argon or xenon) to initiate the deposition process. Advantageously, the heating assembly of the present disclosure provides improved performance, such as heating time, energy efficiency, and geometric size constraints, thereby allowing the system 1100 to be miniaturized and integrated into the charged particle beam system of the present disclosure. In addition, the composition of the deposited material 1140 can be adjusted by adjusting the operation of the heating assembly 1125 (e.g., by adjusting the current directed through the film 1127). In some embodiments, detector data 1145 can be generated based on the interaction of the charged particle beam 1135 with the deposition substrate 1130 (e.g., secondary electrons 1147), which can be used to control the deposition process.

[0079] The system 1100 enables chemical vapor deposition using precursor materials that cannot be delivered to the vicinity of the deposition substrate 1130 using standard equipment for gas delivery (e.g., a gas injection needle system), at least in part due to the tendency of such materials to condense in delivery lines and other surfaces at relatively low temperatures (typically at room temperature or below 200° C.). Precursor materials such as perovskites, tellurium, selenides, sulfur, and other materials can be placed near the deposition substrate 1130 and heated to induce evaporation and / or sublimation. To this end, a heater 1125 for the precursor material 1120 can be maintained at a higher temperature than the temperature of the deposition substrate 1130 (typically in the range of about 400° C. to about 1500° C.). The deposition substrate 1130 can be heated to a temperature between about 100° C. and about 1200° C.

[0080] Thermal radiation generated by the heating assembly 1125 (which may be the hottest part of the system 1100) may impair the performance of SEM detectors (155, 160, 175), which may be sensitive to IR radiation and light emitted by heated parts. The heating assembly 1125 may be configured to minimize the power required for vaporization of the precursor material. For example, using Figure 6 7 to localize heating near the precursor material 1120. When at least a portion of the isolation chamber 1110 (e.g., a cover portion) can be removed to allow the FIB or manipulator needle used for shaping to access the heater 1125, heater shaping is possible before an in-situ vapor deposition experiment, before the precursor material 1120 is placed on the heater 1125 (e.g., in the case of performing precise sample placement) and / or after. In some cases, some of the thermal radiation generated by the heating assembly 1125 can be absorbed by the deposition substrate 1130, thereby affecting the local temperature and heating control stability. Advantageously, the heating assembly of the present disclosure is characterized in that thermal radiation that is approximately an order of magnitude lower (e.g., dissipating approximately 4W instead of approximately 40W for a typical overall heating stage) affects the temperature of the deposition substrate 1130 to a significantly lesser extent, thereby improving the accuracy, stability and precision of thermal control of the deposition substrate 1130.

[0081] In the foregoing description, various embodiments have been described. For the purpose of explanation, specific configurations and details have been set forth in order to provide a thorough understanding of the embodiments. However, it will also be apparent to those skilled in the art that these embodiments can be practiced without these specific details. In addition, in order not to obscure the described embodiments, well-known features may have been omitted or simplified. Although the example embodiments described herein are centered around charged particle beam systems, and particularly around electron microscopy systems, these are meant to be non-restrictive exemplary embodiments. The embodiments of the present disclosure are not limited to such embodiments, but are intended to address analytical instrument systems for which a wide range of material samples can be analyzed to determine chemical, biological, physical, structural or other properties, as well as other aspects for which temperature dependence is of interest.

[0082] Some embodiments of the present disclosure include a system having one or more data processors and / or logic circuits. In some embodiments, the system includes a non-transitory computer-readable storage medium containing instructions that, when executed on the one or more data processors and / or logic circuits, cause the one or more data processors and / or logic circuits to perform part or all of one or more methods disclosed herein and / or part or all of one or more processes and workflows. Some embodiments of the present disclosure include a computer program product tangibly embodied in a non-transitory machine-readable storage medium, the computer program product including instructions that are configured to cause one or more data processors and / or logic circuits to perform part or all of one or more methods disclosed herein and / or part or all of one or more processes.

[0083] The terms and expressions employed herein are used as terms of description and not of limitation, and in the use of such terms and expressions, there is no intention to exclude any equivalents of the features shown and described or portions thereof, but it is to be recognized that various modifications are possible within the scope of the claims. Therefore, it should be understood that while the present disclosure includes particular embodiments and optional features, modifications and changes to the concepts disclosed herein may be made by those skilled in the art, and such modifications and changes are considered to be within the scope of the appended claims.

[0084] When a term is used without explicit definition, it is understood that unless the term has a special and / or particular meaning in the field of charged particle microscopy systems or other related fields, the term is intended to be used in its ordinary sense. The term "about" or "substantially" is used to indicate a deviation from a stated property, wherein the deviation has little or no effect on the corresponding function, property, or attribute of the structure being described. In the illustrated example where one dimensional parameter is described as being "substantially equal to" another dimensional parameter, the term "substantially" is intended to reflect that the two parameters being compared may not be equal within permissible limits (such as manufacturing tolerances or confidence intervals inherent in system operation). Similarly, where a geometric parameter (such as alignment or angular orientation) is described as being "approximately" perpendicular, "substantially" perpendicular, or "substantially" parallel, the term "about" or "substantially" is intended to reflect that the alignment or angular orientation may differ from the precisely stated condition (e.g., not precisely perpendicular) within permissible limits. For numerical values ​​(such as diameter, length, width, etc.), the term "about" may be understood to describe a deviation of up to ±10% from the stated value. For example, a size of "about 10 mm" may describe a size from 9 mm to 11 mm.

[0085] This description provides exemplary embodiments and is not intended to limit the scope, applicability or configuration of the present disclosure. On the contrary, the subsequent description of the exemplary embodiments will provide enabling descriptions for realizing various embodiments to those skilled in the art. It should be understood that, without departing from the spirit and scope set forth in the appended claims, various changes may be made to the function and arrangement of the elements. Specific details are given in the description to provide a thorough understanding of the embodiments. However, it should be understood that the embodiments may be put into practice without these specific details. For example, specific system components, systems, processes and other elements of the present disclosure may be shown in schematic form or omitted from the diagram to avoid obscuring the embodiments due to unnecessary details. In other cases, well-known circuits, processes, components, structures and / or technologies may be shown without unnecessary details.

Claims

1. A heating assembly, comprising: a membrane comprising a carbon nanotube material; a support mechanically coupled to the membrane, the support configured to be integrated with a charged particle beam system; and A heating circuit is electrically coupled to the membrane and configured to direct an electrical current through the membrane. 2 . The assembly of claim 1 , wherein the membrane defines a shape comprising a cone, the cone being defined in a plane in a Cartesian coordinate space.

3. The assembly of claim 2, wherein the shape comprises a bi-conical shape in the plane such that a central region of the membrane is narrower than a peripheral region of the membrane.

4. The assembly of claim 1, wherein the heating assembly is configured to be operably coupled to a sample stage of the charged particle beam system and to position a sample on the heating assembly.

5. The assembly of claim 1, wherein the support comprises a conductive portion in electrical contact with the membrane and electrically coupled to the heating circuit, the heating circuit being configured to direct the current through the membrane via the conductive portion.

6. The assembly of claim 1, wherein the support is configured to operably couple with an electron microscope sample holder. 7 . The assembly of claim 1 , wherein the heating circuit comprises a probe configured to electrically couple with the membrane or the support.

8. The assembly of claim 7, wherein the probe is a first probe, and wherein the heating circuit further comprises a second probe reversibly coupled to the membrane such that the current is directed from the first probe to the second probe via the membrane.

9. The assembly of claim 1, wherein the membrane is at least partially freestanding across an aperture defined in the support.

10. The assembly of claim 1, wherein the carbon nanotube material comprises a multi-walled carbon nanotube mat.

11. The assembly of claim 1 , wherein the membrane comprises multiple layers of carbon nanotube material.

12. A charged particle beam system, comprising: charged particle beam sources; a sample chamber coupled to the charged particle beam source; and A heating component is provided in the sample chamber, and the heating component comprises: a membrane comprising a carbon nanotube material; a support mechanically coupled to the membrane, the support reversibly coupled to a sample stage of the charged particle beam system, and configured for disposing a sample on the support and irradiating with the charged particle beam generated by the charged particle beam source; and A heating circuit is electrically coupled to the membrane and the charged particle beam system and is configured to direct an electric current through the membrane.

13. The charged particle beam system of claim 12, wherein the support comprises a conductive portion electrically coupled to the membrane and to the heating circuit, the heating circuit configured to direct the current through the membrane via the conductive portion.

14. The system of claim 12, wherein the support is configured to mechanically couple with an electron microscope sample holder.

15. The system of claim 12, wherein the heating circuit comprises a probe electrically coupled to the conductive portion of the support or the membrane.

16. The system of claim 12, further comprising an isolation chamber comprising a fluid handling coupling and a deposition substrate, wherein the heating assembly is disposed in the isolation chamber between the fluid handling coupling and the deposition substrate.

17. A method for heating a sample, the method comprising: directing an electrical current through a membrane of a heating assembly, the heating assembly comprising: the membrane, the membrane comprising a carbon nanotube material, the sample being disposed on the membrane; a support mechanically coupled to the membrane, the support reversibly coupled to a sample stage of a charged particle beam system; and A heating circuit is electrically coupled to the membrane and the charged particle beam system and is configured to direct an electric current through the membrane.

18. The method of claim 17, wherein directing the current through the membrane comprises: A power of about 30 W or less is applied through the membrane.

19. The method of claim 17, wherein the membrane has a sample disposed thereon, the method further comprising: removing material from the membrane in a region of the membrane that is peripheral to the sample; as well as The membrane is brought into contact with a probe within the region of the periphery of the sample, the probe being electrically coupled to the heating circuit.

20. The method of claim 19, wherein removing the material comprises: The film is irradiated using a charged particle beam.

Images