Improved x-ray analysis of heated samples in electron microscopes

Abstract

A system for energy dispersive X-ray analysis of a sample in a particle beam instrument is provided, the system comprising an X-ray detector 5 and a filter member, the system being adapted such that, in a first mode of operation, the filter member and the detector are positioned to provide an unobstructed line of sight between the sample and the detector, and, in a second mode of operation, the filter member and the detector are positioned to provide an unobstructed line of sight between the sample and the detector. And in a second mode of operation, the filter member and the detector are positioned to block a line of sight between the sample and the detector such that, in use, the proportion of blackbody radiation emitted from the sample incident on the detector is attenuated.

Description

Technical Field

[0001] The present invention relates to a system for improved X-ray analysis of a sample in an electron microscope. Background Art

[0002] The properties of metallic materials vary depending on temperature and mechanical stress. Analyzing these materials when subjected to varying temperatures helps understand phenomena from precipitation to phase transformations, and thus allows metallurgists and materials scientists to develop new materials with better properties. X-ray analysis using characteristic X-ray emission from an energy dispersive spectrometer (EDS) can be used for in-situ heating analysis inside an electron microscope (EM), and more specifically for dynamic in-situ experiments where phenomena such as precipitation or phase transformations can be observed in real time.

[0003] Figure 1 A simplified view of a system for X-ray analysis of heated samples in an electron microscope is shown. It is the same application as described in US10656106B2. Figure 1 The system comprises a vacuum sample chamber 100 defined by a wall 101 in which a vacuum is obtained during use. During use, a sample 102 is mounted on a stage so that an incident electron beam 104 excites characteristic X-rays 112 from the sample 102. The characteristic X-rays 112 are measured by an X-ray detector tube 114 inserted through a port on the vacuum chamber wall 101.

[0004] Figure 2 A schematic cross section of an EDS detector commonly used for X-ray detection is shown. For heating experiments, the stage may use a heating element, or heat may be generated by other means, such as focusing a laser beam on the sample 102, and the sample temperature may typically increase to over 100°C, but may be 1500°C or even higher depending on the research needs. However, if the temperature exceeds 150°C, some components within most types of EDS detectors may be damaged, so when the sample 102 is heated to much higher than 150°C, the EDS detector cannot have any significant thermal connection with the sample. Therefore, for this type of application, the sample chamber is evacuated to a vacuum 100 at a sufficiently low pressure to ensure that thermal conductivity by convection is negligible. In this case, the detector is only exposed to thermal (blackbody) radiation 122 from the sample 102 and the stage, and if this radiation energy can be dissipated by conduction through the detector body, the temperature of the EDS detector components can be kept well below 150°C even when the sample 102 is heated to a much higher temperature.

[0005] EDS analysis in EM is usually performed at room temperature, with the sample and detector in a vacuum environment. Even though there is no convection or conduction of heat through a vacuum, operation on high temperature samples is more challenging because the black body radiation (IR, visible and UV) emitted from the heating device has a huge impact on the quality of the recorded X-ray spectrum. At high temperatures (>600°C), the signal is degraded by noise effects caused by the black body radiation from the sample, so it becomes impossible to collect a useful spectrum.

[0006] like Figure 2 As shown, a conventional EDS detector has a window 232 that provides a barrier to seal the vacuum 200 inside the detector while being as transparent to X-rays as possible. Characteristic X-rays 212 from the sample 102 and blackbody radiation 222 from the sample 102 and the stage enter the detector through an entrance collimator 228 in the detector housing, which faces the sample. The characteristic X-rays 212 from the sample 102 and the blackbody radiation 222 from the sample 102 and the stage then impinge on a sensor material 234, which typically includes a semiconductor such as silicon. The detector also includes cooling elements and front-end electronics for the sensor 236, and a magnetic electron trap 230 configured to prevent electrons from reaching the window 232. A reflective layer 238 of typically 40 nm aluminum is typically included in the window structure to block the weak visible light emitted when the cathodoluminescent (CL) sample is hit by the electron beam. Most samples are not CL, but any sample emits blackbody radiation. If the sample is heated, the intensity of this blackbody radiation will increase, and the spectral distribution of the thermal radiation also changes with temperature, such as Figure 3 An electron trap is not always necessary if the EM electron optics direct the backscattered electrons away from the entrance collimator.

[0007] The EDS detector system produces a voltage ramp at the output. Each X-ray photon detected by the detector produces a voltage step on the ramp that is proportional to the photon energy, and the step height is measured by the electronics. However, visible photons have much less energy than X-ray photons and do not produce a measurable step on the ramp, but they cause an increase in the slope gradient, so the slope gradient is an indication of how much light is reaching the EDS detector.

[0008] An EDS detector fitted with a standard window with a reflective coating of only 40nm of aluminium will be sensitive to radiation from the heated sample. Figure 4 It is shown that when the temperature exceeds 560°C (833K), there is a considerable increase in the slope gradient detected by a typical EDS detector. Figure 3As shown, depending on the temperature, the photons of black body radiation emitted from the sample are mainly in the infrared wavelength range, the visible light range or the ultraviolet wavelength range, and the heating temperature of 833K (560°C) is approximately the temperature at which visible light radiation (wavelength of 0.4μm to 0.8μm) begins to be emitted. Therefore, Figure 4 The increase in the ramp gradient shown in indicates that the EDS detector used is more sensitive to visible light than to longer wavelength emission. The increase in the ramp gradient produces an undesirable effect equivalent to excess electronic noise, resulting in a degradation of the resolution of the X-ray spectrum, making characteristic emission peaks more difficult to separate, and at certain temperatures, the spectrum may no longer be useful for X-ray analysis. At this point, the X-ray detector is said to be saturated.

[0009] This problem has been solved in US10656106B2, where, in order to reduce degradation and make EDS usable at high temperatures, a much thicker aluminum layer is used as coating 238 to more effectively block blackbody radiation. For example, a silicon nitride film is used for window 232, and the thickness of its aluminum coating 238 ranges between 50nm and 400nm. Torma et al. (IEEE Trans. Nuclear Science, vol60no 2April 2013, 111) describe a "solar blind" window that, when mounted to an EDS detector, allows it to operate in daylight. A commercial product C1 from Amptek uses 150nm Si3N4 with a 250nm aluminum coating for indoor light: (https: / / www.amptek.com / products / x-ray-detectors / fastsdd-x-ray-detectors-for-xrf-eds / c-series-low-energy-x-ray-windows). These "solar blind" windows were not originally intended for use in EM, but were designed for X-ray fluorescence studies, where the sample is excited by an X-ray tube source of X-rays under daylight conditions. Using an aluminum coating with a thickness much greater than 40 nm will reduce blackbody radiation during heating experiments, but has the disadvantage of reducing X-ray transmission (especially for low energy X-rays). While this reduction in performance for low energy X-rays may be an acceptable sacrifice to allow data to be acquired at high sample temperatures, it is undesirable when the detector is used for routine analysis of unheated samples.

[0010] For studies that require heating samples to very high temperatures, new problems arise. Figure 3As shown, not only has the power of the radiation increased by several orders of magnitude, but an increased proportion of radiation has also appeared in the visible or UV region of the spectrum, so any filter must be able to block photons with increasingly higher energy (shorter wavelengths). The increased radiation load on the detector will cause the material to heat up. In order to maintain the vacuum within the detector sensor package, the window must form a seal with the detector housing, which is inevitably achieved by gluing, soldering or welding. A series of materials, windows, support grids, window mounts, detector housings, and any glue or solder have different thermal expansion coefficients, so that the radiation load increases, the temperature rises, the mechanical stress increases, and mechanical or chemical decomposition may occur, causing the window to be damaged. Therefore, the detector may only be able to function under conditions where the window temperature is below 150°C. This constraint limits the distance at which the detector can approach the sample (to collect a stronger X-ray signal) and the temperature at which the sample can be heated without damaging the detector.

[0011] A better solution for X-ray spectroscopy of samples inside electron microscopes is needed that can allow analysis at very high temperatures (e.g., >600° C.) without significantly compromising X-ray detector sensitivity for studies that do not require heating of the sample. Summary of the invention

[0012] According to a first aspect of the invention, there is provided a system for energy dispersive X-ray analysis of a sample in a particle beam instrument, the system comprising an X-ray detector and a filter member, the system being adapted such that in a first operating mode, the filter member and the detector are positioned to provide an unobstructed line of sight between the sample and the detector, and in a second operating mode, the filter member and the detector are positioned to block the line of sight between the sample and the detector,

[0013] Such that, in use, the proportion of blackbody radiation emitted from the sample that is incident on the detector is attenuated.

[0014] It has been found that employing a system having such a configuration can provide significant improvements to EDS analysis of a sample. First, the system can be easily switched between two different operating modes, wherein the first mode provides an unobstructed line of sight between the sample and the detector in order to maximize X-ray detection sensitivity, and the second mode has a line of sight blocked by a filter member such that in the second operating mode, blackbody radiation emitted from the sample and other heated components of the system is attenuated. Following the theory provided in the Background section above, employing a system having such a configuration is particularly useful in applications where analysis of both heated and room temperature samples is to be performed.

[0015] The second operating mode can be used for EDS analysis of heated samples to attenuate the proportion of black body radiation incident on the detector, thereby reducing the reduction in resolution of the X-ray spectrum so that characteristic emission peaks can still be identified and separated. The point at which the X-ray detector can no longer output a meaningful system for EDS analysis may be referred to herein as the X-ray detector becoming saturated. Therefore, the second operating mode of the system is employed when used to analyze heated samples to prevent the black body radiation from saturating the X-ray detector.

[0016] The first operating mode may be used to perform EDS analysis on room temperature samples to maximize the sensitivity of the X-ray detector when blackbody radiation is negligible.

[0017] It should be understood that in the context of the present disclosure, a particle beam instrument can be considered to be a device configured to generate a focused particle beam (e.g., an electron beam) that serves as an X-ray excitation source to perform energy dispersive X-ray analysis of a sample. The detector sensor area can typically be 10 mm 2 Up to 170mm 2 The filter components are usually designed to fit the area of ​​the sensor used.

[0018] Typically, the X-ray detector is a semiconductor X-ray detector and includes a sensor element that can be used to monitor the energy of X-ray photons. The area including the sensor element may be referred to herein as the active area of ​​the X-ray detector. The sensor may be adapted to measure, or otherwise provide or output a signal or data representing the detection or energy of received X-ray photons. Thus, the sensor element may be configured to detect a single received X-ray photon and monitor the energy of a single received X-ray photon.

[0019] In all aspects of the present disclosure, the term "filter member" is intended to mean a component or group of components of a system that is suitable for filtering electromagnetic radiation, and in particular, filtering electromagnetic radiation corresponding to blackbody radiation emitted from a heated sample, particularly electromagnetic radiation in the infrared band, the visible light band, and the ultraviolet band. The filter member may also additionally attenuate radiation originating from the cathode-ray luminescence of the cathode-ray luminescent sample, typically radiation in the visible light band. The filter member includes a filter material having a suitable composition and geometry so that the filter member provides a wavelength-dependent attenuation distribution of the incident electromagnetic radiation. Although certain specific examples of compositions and geometries are described in detail below, it will be understood that other compositions and geometries that exhibit suitable wavelength-dependent attenuation distributions may be employed based on the desired application.

[0020] In all aspects of the present disclosure, the filter member may be referred to as a filter assembly alternatively. The filter member or assembly may include one or more components, which include filter material. The filter material is usually provided in the form of a film, a membrane or a window member including the material. The filter material may be included in a filter material element, which is a component of the filter member and includes a filter material and a supporting structure or a supporting element, such as a ring or a frame in which the filter material is installed or fixed, so that the filter window is manipulated. The filter material element may also include a support grid, on which the filter material is arranged.

[0021] "First operating mode" and "second operating mode" are intended to refer to operating modes in which the system can be used to perform EDS analysis. In particular, the two modes may refer to two different configurations in which the system can operate, wherein the positioning of at least one of the X-ray detector and the filter member is different between the two modes. When referring to the positioning of the X-ray detector and the filter member, the term "positioning" will be understood to refer to the relative positioning of the X-ray detector and the filter member with respect to each other. The first operating mode is typically employed when analyzing room temperature samples, and the second operating mode is typically employed when analyzing heated samples.

[0022] In the first operating mode, an unobstructed line of sight between the filter member and the active area of ​​the detector is provided by the relative positioning of the detector and the filter member. This can be considered as providing at least one unobstructed line of sight between a portion of the sample and the active area of ​​the detector, thus including a filter member that partially blocks the detector from some parts of the sample. Preferably, in the first operating mode, multiple lines of sight between a portion of the sample and the active area of ​​the detector are unobstructed in the first operating mode so as to provide an unobstructed solid angle within which all lines of sight are unobstructed.

[0023] Preferably, in the first operating mode, all sight lines between the sample and the active area of ​​the X-ray detector are unobstructed. In other words, in this configuration, portions of the sample are not blocked by the filter member, which advantageously allows unrestricted visibility or access to the location of incidence of the particle beam and prevents absorption of low energy X-rays emitted from the sample, maximizing the sensitivity of the detector for X-ray detection.

[0024] In the second operating mode, the relative positioning of the detector and the filter member is such that the unobstructed line of sight provided between the filter member and the active area of ​​the detector in the first operating mode is blocked. In other words, in the second operating mode, the filter member blocks a greater proportion of the sample from the detector than in the first operating mode. However, it will be understood that in the second operating mode, the filter member may still partially block the detector from some portions of the sample.

[0025] Preferably, in the second operating mode, all lines of sight between the sample and the active area of ​​the X-ray detector are blocked. In other words, in this configuration, all parts of the sample are blocked by the filter member so that the attenuation of the black body radiation emitted from the sample is maximized, thereby minimizing its impact on the resolution of the X-ray analysis. This can be achieved, for example, by configuring the system to position the filter member above the entrance collimator of the X-ray detector in the second operating mode.

[0026] The system can be operated in the first operating mode or the second operating mode by changing the relative positioning of the X-ray detector and the filter member by moving at least one of the detector and the filter member, so that the proportion of the effective sensor area of ​​the detector blocked by the filter member changes.

[0027] In some examples, the filter member may be movable between a first position relative to the detector corresponding to the first operating mode and a second position relative to the detector corresponding to the second operating mode. In these examples, the X-ray detector may be located at the same position in the first operating mode and the second operating mode. As an alternative or supplement to the above-mentioned features, the detector may be movable between a first position relative to the filter member corresponding to the first operating mode and a second position relative to the filter member corresponding to the second operating mode. In these examples, the filter member may be located at the same position in the first operating mode and the second operating mode. In the above two groups of examples, the relative positioning of the detector and the filter member may be adapted to enable the system to work in the first operating mode and the second operating mode during use.

[0028] In some examples, the system is adapted so that in a first operating mode, the detector is closer to the sample than in a second operating mode. Advantageously, positioning the detector closer to the sample in the first operating mode increases the solid angle for collecting X-rays, while positioning the detector farther from the sample in the second operating mode reduces the incident power of blackbody radiation emitted from the sample on the detector, thereby reducing the amount of attenuation that needs to be provided by the filter member in order to obtain a spectrum useful for X-ray analysis.

[0029] In some examples, the system includes a mounting element, the mounting element includes an opening, and the filter member can be removably attached to the mounting element on / across the opening. "Mounting element" can be understood as a component of the system that is suitable for accommodating the filter member, so that when installed, the filter member at least partially covers the opening. The mounting element can be, for example, a baffle or a shutter mechanism.

[0030] In a preferred example, the mounting element is movable between a first position relative to the detector corresponding to the first operating mode and a second position relative to the detector corresponding to the second operating mode. The mounting element may be implemented as a baffle attached to the housing of the system at a first point such that the baffle is movable about the attachment point. In this way, the proportion of the active area of ​​the detector that is blocked by the filter member can be changed by movement of the mounting element so that the system can simply change between operation in the first operating mode and the second operating mode.

[0031] In order to allow movement of the mounting element and provide consistent first and second positions corresponding to the two operating modes, in some examples, the mounting element is biased toward the second position by a resilient biasing element, wherein the biasing element is typically a spring tension mechanism. The spring tension mechanism is typically configured to hold the mounting element in the second position. A force is then applied to the mounting element by the system to actuate the mounting element to move from the second position to the first position. Alternatively, the mounting element can be supported on a hinge, wherein the mounting element and the hinge are adapted so that gravity holds the mounting element in the second position. A force is then applied to the mounting element by the system to actuate the mounting element to move from the second position to the first position.

[0032] Actuating movement of the mounting element between the first position and the second position can be performed manually, under motorized control, or by another component of the system. In some examples, the system further includes a motor, wherein the motor is configured to actuate movement of the mounting element between the first position relative to the detector and the second position relative to the detector. In this way, the mounting element can be conveniently repositioned between the first position and the second position to switch between the first operating mode and the second operating mode.

[0033] Alternatively, movement of the mounting element may be actuated by movement of another component of the system. In some examples, the X-ray detector is mounted to a support arm that is movable along a mechanical slide between a first position relative to the filter member and a second position relative to the filter member, such that movement of the support arm from the second position toward the sample to the first position actuates movement of the mounting element between the second position and the first position.

[0034] Typically, when the mounting element is implemented as a baffle as described above, movement of the support arm toward the sample causes a portion of the support arm to contact the mounting element and provide a force that actuates the mounting element to move from the second position to the first position. In the case where the mounting element is biased toward the second position, the contact force resists the bias of the mounting element. Equivalently, when the support arm is retracted from the first position away from the sample to the second position, the bias of the mounting element in the absence of the contact force causes the mounting element to return to the second position.

[0035] In some examples, the system further comprises a shutter mechanism configured to move the filter member or a component of the filter member between a first position relative to the detector corresponding to the first operating mode and a second position relative to the detector corresponding to the second operating mode. A "shutter mechanism" may be understood as a component adapted to change the proportion of an active area of ​​the X-ray detector that is blocked by the filter member, such that the system may be changed between the first operating mode and the second operating mode by actuating the shutter mechanism, thereby providing a convenient means of switching the system between the operating modes.

[0036] In some examples, the filter member is configured to keep the filter material element in place by at least one of friction fit, clearance fit and transition fit. Advantageously, a filter member is provided, wherein the thermal expansion and contraction of the filter material element are adapted, i.e., by allowing the filter material element to be changed relative to one or more other parts of the filter member (e.g., relative to its filter cover) in size, position and one or more dimensions, without generating mechanical stress in the filter material (if the element adheres or otherwise is fixed to the filter member in a non-yielding manner, mechanical stress will occur). Because the filter member is suitable for analysis involving variable temperatures, the inventor has found that this arrangement for holding the filter material element enables the element to experience a significantly greater number of thermal cycles before it needs to be replaced, wherein, in this arrangement, the destructive thermal expansion effect is mitigated.

[0037] In some examples, filter member also comprises removable cover, and this removable cover is suitable for being installed to system, and filter member is configured so that filter material element is removably installed to removable cover.Filter material element can be directly installed to removable cover, or can be installed indirectly via the parts of filter member or assembly fixed with filter material element or otherwise coupled, wherein filter material element is usually set to window element.Usually, cover comprises opaque material and opening, and filter material is preferably removably installed, makes in use, filter material is arranged on opening / through beginning arrangement.In these examples, because filter member is removably attached to mounting element, filter member or filter material element can be easily replaced or replaced for example in the case of damage.

[0038] In some examples of any one of the aspects set forth in the present disclosure, filter member comprises elastic element, and this elastic element is suitable for making in use, elastic element applies force on filter material element, makes filter material be kept in place.Filter member or assembly can be arranged so that elastic element directly applies force on filter material, or for example, applies force indirectly on filter material by contact between elastic element and filter material element or filter member or assembly and filter material window or other filter material element fixed or otherwise coupled parts.In these examples, because filter material is kept in place by elastic element instead of being glued, welded, so filter member can withstand higher head load (head loads), because its free thermal expansion or contraction and there is no additional mechanical stress observed in glue, welded joint.In the preferred example of this arrangement, filter member comprises front cover part, spring element, back cover part and the threaded fitting for front cover part being attached to back cover part, wherein filter member is configured so that when front cover part and back cover part are screwed together, filter material element can be kept in place by friction against spring element. In this way, the filter material element is not only free to expand and contract thermally but can also be easily replaced, for example in the event of damage.

[0039] In some examples, filter member comprises the groove that is suitable for accommodating filter material element, makes filter material element and filter member form clearance fit.Should be appreciated that filter member can be suitable for directly accommodating filter material element, perhaps indirectly accommodating filter material element via the parts of filter member or assembly, filter material window or other filter material elements are fixed or otherwise coupled to the described parts of filter member or assembly.In these examples, the inner surface of the groove of filter member can comprise one or more guide elements, and described guide element is suitable for helping filter material element to be centered on the opening of filter member.In some examples, filter material element can be further fixed in the appropriate position on the opening by clamping plate or screw.

[0040] In some examples, the filter member also includes a magnetic electron trap. Typically, the magnet is closer to the sample than the filter material element so that any backscattered electrons from the sample are captured before they can excite any X-rays from the filter material. It should be understood that an electric field or a combination of a magnetic field and an electric field may be used alternatively to provide the functionality of the magnetic electron trap described above. In a preferred example, the filter member is adapted so that the filter material element can be inserted into the space between the electron trap and the detector. The filter material element may be directly insertable or may be inserted indirectly via a component of the filter member or assembly that is fixed to or otherwise coupled to a filter material window or other filter material element. This may be accomplished manually or using a filter material element on a motorized slide. This arrangement avoids excitation of X-rays from the filter material and allows the use of the same electron trap regardless of whether the filter material element is inserted into or removed from the space in the filter member.

[0041] In some examples, the filter member comprises a window member, and this window member comprises filter material or is formed by filter material.Preferably, the average thickness of the filter material along the direction between sample and detector of window member or its back is greater than or equal to 100nm." thickness " here will be understood to refer to total average thickness, for example, if the filter member comprises multiple layers, then comprises all layers of filter material.It has been shown that when carrying out the analysis of heated sample, mainly depends on the selection and sample temperature of filter material, and the thickness of 100nm to 1000nm is suitable.It is to be understood that this window member, also can be considered as filter material window or filter membrane, is preferably provided as the filter material element with supporting structure or element, for example, ring or framework of filter material are installed or fixed, so that operation filter window.

[0042] In some examples, the filter member includes any one or more of silicon nitride, polymer, aluminum, beryllium, carbon, or graphene. It has been shown that these materials, when arranged in appropriate geometries and / or combinations, achieve the desired attenuation of blackbody radiation, improving the resolution of X-ray spectroscopy when analyzing heated samples.

[0043] Specifically, in some examples, the filter member comprises silicon nitride or a polymer having a coating of at least 200 nm of aluminum, or beryllium foil. Alternatively, in some examples, the filter member comprises carbon or multilayer graphene, wherein the average thickness along the direction between the sample and the detector is between 100 nm and 1000 nm. It has been shown that the combination of these materials and geometries achieves the desired attenuation of blackbody radiation, improving the resolution of X-ray spectra when analyzing heated samples.

[0044] According to a second aspect of the present invention, there is provided a method for performing energy dispersive X-ray analysis of a sample based on a first operating mode of a system according to the first aspect or any embodiment of the first aspect, the method comprising: positioning the sample on a sample stage within a sample chamber of the system; generating a focused particle beam using a particle beam assembly; and monitoring the energy of X-ray photons generated by the interaction between the particle beam and the sample using an X-ray detector.

[0045] The method according to the second aspect involving operating the system in the first operating mode may be used to perform EDS analysis on room temperature or cold samples to maximize the sensitivity of the X-ray detector.

[0046] Preferably, after positioning the sample, the sample chamber may be evacuated such that the pressure within the chamber is lower than ambient pressure.

[0047] The advantages associated with the different embodiments of the first aspect are the same and applicable to the second aspect described above.

[0048] According to a third aspect of the present invention, there is provided a method for performing energy dispersive X-ray analysis on a sample based on a second operating mode of a system according to any one of claims 1 to 25, the method comprising: positioning the sample on a sample stage within a sample chamber of the system; heating the sample to a temperature greater than or equal to 100°C; generating a focused particle beam using a particle beam assembly; and monitoring the energy of X-ray photons generated by the interaction between the particle beam and the sample using an X-ray detector.

[0049] The method according to the third aspect involving operating the system in a second operating mode can be used to perform EDS analysis of a heated sample to attenuate the proportion of blackbody radiation incident on the detector and reduce the reduction in resolution of the X-ray spectrum so that characteristic emission peaks can be identified and separated.

[0050] Preferably, after positioning the sample, the sample chamber may be evacuated such that the pressure within the chamber is lower than ambient pressure.

[0051] The advantages associated with the different embodiments of the first aspect are applicable to the third aspect described above.

[0052] In a preferred example of the third aspect, heating the sample to a temperature of 100° C. or more further comprises heating the sample to a temperature of 600° C. or more. In other examples, heating the sample to a temperature of 100° C. or more further comprises heating the sample to a temperature of 1500° C. or more. It has been shown that employing the system according to the first aspect enables successful EDS analysis of heated samples at these temperatures.

[0053] In a fourth aspect of the present invention, a filter component suitable for attachment to a system for performing energy dispersive X-ray analysis of a sample is provided, the filter component being removably attached to the system at a position between the sample and a detector of the system, the filter component comprising a filter material element, and being configured to hold the filter material element in place by at least one of a friction fit, a clearance fit, and a transition fit.

[0054] Advantageously, a filter member is provided in which thermal expansion and contraction of a filter material element is accommodated, i.e., by allowing any of the size, position, and one or more dimensions of the filter material element relative to one or more other parts of the filter member (e.g., relative to its filter cover) to be changed without generating mechanical stresses in the filter material (which would occur if the element were adhered or otherwise fixed to the filter member in a non-yielding manner). Since the filter member is suitable for analysis involving varying temperatures, the inventors have found that such an arrangement for retaining the filter material element enables the element to undergo a significantly greater number of thermal cycles before it needs to be replaced, wherein in this arrangement, the destructive thermal expansion effects are mitigated.

[0055] In some examples, the filter component included by the system of the first aspect is a filter component according to the fourth aspect.

[0056] In some examples, the filter member comprises a removable cover. It may be configured such that the filter material element is removably mounted to the removable cover.

[0057] By using a filter assembly in which the filter material element is removably mounted rather than glued or welded, the filter assembly can withstand higher head loads because it is free to thermally expand or contract without causing additional mechanical stresses as observed in glued or welded joints. This allows the filter assembly to be positioned closer to the heated sample, and it has been found that the filter assembly is typically located almost 20 mm from the sample.

[0058] In some examples, the filter material element is removably mounted to the removable cover by an interference fit, and is removably mounted to any one or more parts of the filter member. In this way, the filter element is fastened to its installation position in the filter member so that it is maintained by friction (preferably, replacing bonding, welding or other types of more immovable fixing methods), which alleviates the problem of material strain and stress that would otherwise be caused to the filter material due to thermal expansion and contraction. In a preferred example, the filter material element remains on its installation position without any adhesive or similar permanent connection, and more preferably only maintained by friction.

[0059] In some examples, the filter member comprises a resilient element adapted such that, in use, the resilient element exerts a force on the filter material element such that the filter material is held in place.

[0060] The filter component or assembly can be arranged so that the elastic element exerts a force directly on the filter material, or indirectly, for example through contact between the elastic element and a filter material element or a part of the filter component or assembly that is fixed or otherwise coupled to a filter material window or other filter material element.

[0061] In all aspects of the present disclosure, "elastic element" will be understood as being suitable for providing parts of restoring force when deforming from its equilibrium state or when displacing from its equilibrium position.Usually, restoring force is provided at one or more contact points between elastic element and filter material or filter material element, wherein restoring force is generated by compression of elastic element at the contact point with filter material or filter material element, filter material or filter material element itself contacts with the housing of filter member or assembly at the opposite face.Like this, friction is maintained at filter material in place.Filter member or assembly can be arranged so that elastic element directly applies force on filter material, or for example, applies force indirectly on filter material by contact between parts that are fixed or otherwise coupled with filter material window or other filter material elements of elastic element and filter member or assembly.

[0062] In some examples, the filter member is suitable for making the filter material element and the filter member form a clearance fit. This again allows the filter material element to expand or contract freely without causing additional mechanical stress. In some examples, the filter member includes a groove suitable for accommodating the filter material element so that the filter material and the filter member form a clearance fit. It should be understood that the filter member can be suitable for directly accommodating the filter material element, or indirectly accommodating the filter material element via the filter member or the component of the assembly, wherein the filter member or the component of the assembly is fixed to or otherwise coupled to the filter material window or other filter material element. In these examples, the inner surface of the groove of the filter member may include one or more guide elements, which are suitable for helping to center the filter material element on the opening of the filter member. In some examples, the filter material element can be further fixed in the appropriate position on the opening by a clamp or a screw. It can be imagined that the combination of interference fit or friction fit and clearance fit can be used to keep the installed filter material element in the appropriate position. For example, the filter material element can be kept in the mounting element by press fit (pressed fit), and the mounting element can be accommodated by the filter member and can be kept therein by clearance fit. Any of these joints can be realized by any one of clearance fit, transition fit and interference fit. Advantageously, this arrangement avoids potential damage that filter components, particularly filter material elements, may suffer when subjected to heating or cooling.

[0063] The filter material element can be directly mounted to the removable cover, or can be installed indirectly via the parts of the filter member or assembly that are fixed with the filter material window or other filter material elements or otherwise coupled.Usually, the cover comprises an opaque material and an opening, and the filter material is preferably removably mounted on the opening / installed through the opening.In these examples, since the filter member is removably attached to the mounting element, the filter member can be easily replaced or replaced, for example, in the case of damage.In the preferred example of this arrangement, the filter member comprises a front cover part, a spring element, a rear cover part and a threaded fitting for attaching the front cover part to the rear cover part, wherein the filter member is configured so that when the front cover part and the rear cover part are screwed together, the filter material can be kept in place by the friction against the spring element.Like this, the filter material element is not only free to thermally expand and contract, but also easily replaced, for example, in the case of damage.

[0064] In some examples, the filter member also includes a magnetic electron trap. Typically, the magnet is closer to the sample than the filter material elements so that any backscattered electrons from the sample are captured before they can excite any X-rays from the filter material. In a preferred example, the filter member is adapted so that the filter material can be inserted into the space between the electron trap and the detector. The filter material can be directly insertable, or can be inserted indirectly via a component of the filter member or assembly that is fixed or otherwise coupled to the filter material window or other filter material elements. This can be achieved manually or using the filter on a motorized slide. This arrangement avoids excitation of X-rays from the filter material and allows the same electron trap to be used regardless of whether the filter is inserted into or removed from the space in the filter member.

[0065] In some examples, the filter member comprises a window member, which comprises a filter material or is formed by a filter material. Preferably, the average thickness of the filter material along the direction between the sample and the detector of the window member or its back is greater than or equal to 100nm." thickness "here will be understood to refer to the total average thickness, for example, if the filter comprises a plurality of layers, then refers to all layers comprising the filter material. It has been shown that when the analysis of the heated sample is carried out, it depends mainly on the selection and sample temperature of the filter material, and a thickness of 100nm to 1000nm is suitable. It is to be understood that the window member, which may also be considered as a filter material window or a filter film, is preferably provided with a supporting structure or element, for example, a ring or a frame wherein the filter material is installed or fixed, so that the filter window can be operated.

[0066] In some examples, the filter member includes any one or more of silicon nitride, polymer, aluminum, beryllium, carbon, or graphene. It has been shown that these materials, when arranged in appropriate geometries and / or combinations, achieve the desired attenuation of blackbody radiation, improving the resolution of X-ray spectroscopy when analyzing heated samples.

[0067] Specifically, in some examples, the filter comprises silicon nitride or a polymer with a coating of at least 200 nm of aluminum, or beryllium foil. Alternatively, in some examples, the filter comprises carbon or multilayer graphene, with an average thickness between 100 nm and 1000 nm along the direction between the sample and the detector. It has been shown that these combinations of materials and geometries achieve the desired attenuation of blackbody radiation, improving the resolution of X-ray spectra when analyzing heated samples.

[0068] More generally, and in any aspect according to the present disclosure, the filter material element may be adapted (i.e., it may comprise any suitable material and may have any suitable dimensions) to attenuate the proportion of black body radiation emitted from the sample being analyzed that is incident on the detector in use. The degree of attenuation that the filter element is adapted to achieve may be selected based on one or more characteristics of the detector, one or more operating conditions, and / or the sample. BRIEF DESCRIPTION OF THE DRAWINGS

[0069] Examples of the present invention will now be described with reference to the accompanying drawings, in which like features are indicated by like reference numerals, and in which:

[0070] Figure 1 A schematic diagram showing an X-ray analysis of a heated sample in an electron microscope according to the prior art is shown.

[0071] Figure 2 A schematic cross section of a typical EDS X-ray detector according to the prior art is shown.

[0072] Figure 3 The emission curves of blackbody radiation at different temperatures are shown.

[0073] Figure 4 The ramp gradient detected by a conventional EDS detector at different sample temperatures is shown.

[0074] Figure 5 A schematic assembly of an additional filter cover for analysis of heated samples according to an example of the present invention is shown.

[0075] Figure 6 An additional filter cover mounted on an entrance collimator of an X-ray detector according to an example of the present invention is shown.

[0076] Figure 7 An X-ray detector is shown in a second position suitable for analysis of a heated sample according to an example of the present invention.

[0077] Figure 8 An X-ray detector is shown in a first position suitable for measurement without heating a sample specimen according to an example of the present invention.

[0078] Fig. 9 The calculated optical transmission of a 1000 nm thick carbon film compared to a 250 nm aluminum layer is shown.

[0079] Fig.10 X-ray transmission curves of a 1000 nm thick carbon film and a 150 nm silicon nitride film coated with 250 nm aluminum, where the 150 nm silicon nitride film is supported on a thick silicon grid with 80% open space, are shown. DETAILED DESCRIPTION

[0080] With reference to the accompanying drawings, an embodiment of a method according to the present invention is now described, which reduces the effect of blackbody radiation on the EDS detector when the sample is heated to a high temperature (>600°C), preferably a very high temperature (>1000°C), and most preferably an extremely high temperature (>1500°C), without significantly compromising the ability to analyze the sample at room temperature, for example, without reducing low energy sensitivity or spectral peak resolution.

[0081] The example of the system for energy dispersive x-ray analysis of samples in a particle beam instrument described below retains the use of traditional windows with good low energy x-ray transmission to seal the vacuum on the detector, but when the detector is needed to study heated samples, a separate additional filter component is inserted between the detector and the sample. When the additional filter component is in place, it is closer to the sample than the detector and will be subjected to a much higher thermal load than the window on the detector. The additional filter component does not have to form a vacuum seal with the detector housing, and if the additional filter component is damaged, the additional filter component can be replaced without repairing the x-ray detector. In addition, if the additional filter component or any part of the filter component can be kept in place without using glue or solder, the mechanical stress caused by different thermal expansion coefficients can be significantly reduced, so that the additional filter component can work at a higher temperature than the conventional x-ray detector window. The filter component can include a filter material element that can be mounted on a removable cover, and the removable cover is suitable for mounting to the end of the detector housing. Figure 5 One embodiment of such a cover is shown.

[0082] Figure 5 An example of a filter component embodied as a cover 500 is shown, the cover 500 comprising a front cover part 501, a filter material element 502, a spring element 503 and a rear cover part 504. Figure 5 In the embodiment, the filter material element 502 is not glued or welded to the cover 500, but is held in place by friction with the spring element 503 when the front cover part 501 and the back cover part 504 are screwed together. Therefore, the filter material element 502 can expand and contract with changes in temperature without causing any mechanical stress. Therefore, if the filter material itself is stable, the cover 500 can withstand much higher temperatures than if the filter is held in place by glue or welding. Although the spring element 503 is Figure 5 503 is shown as a spring washer, but the spring element 503 may include any elastic element suitable for exerting a force on the filter material element 502 so that the filter material is held in place. It should also be understood that the spring element 503 may be located between the back cover portion 504 and the filter material element 502, such as Figure 5As shown in the exploded view of , or alternatively, it can be located between the front cover part 501 and the filter material element 502.

[0083] In some examples, the filter member may not include the spring element 503, and may be adapted to alternatively keep the filter material element 502 in the proper position in the groove between the front cover part 501 and the back cover part 504 by a clearance fit, so that the filter material element can expand and contract with changes in temperature without causing any mechanical stress. In the case where the spring element 503 is not provided, one or more of the front cover part 501 and the back cover part 504 may include one or more guide elements, which are adapted to help center the filter material element 502 on the opening of the removable cover when the front cover part 501 and the back cover part 504 are screwed together. In other examples, the filter material element 502 may be further fixed in place by a clamp or a screw.

[0084] Figure 6 is a diagram showing an additional filter cover 600 installed on the end of a conventional X-ray detector in preparation for studying a heated sample. For example, the filter cover 600 may be Figure 5 Filter cover 500 shown. Filter cover 600 does not have to be glued or welded to the detector, and the rear cover portion can simply be friction fit onto the end of the entrance collimator. During investigations, the front cover portion can typically be positioned as close as 20 mm to the sample. The detector sensor area can typically be within 10 mm 2 Up to 170mm 2 range, and the filter cover 600 can be designed to adapt to the area of ​​the sensor used. In another variation, the filter cover 600 may include a magnetic electron trap, with the magnet closer to the sample than the filter; in this variation, any backscattered electrons from the sample are captured before they can excite any X-rays from the filter material. In another variation, since the electron trap magnet is outside the detector vacuum, the filter material can be inserted into a slot in the space between the magnet and the detector. This can be achieved manually or using a filter material element on a motorized slide. This arrangement again avoids excitation of X-rays from the filter material, and the same electron trap can be used whether the filter material element is inserted into or removed from the slot.

[0085] When the additional filter member and filter material elements are in place, the black body radiation from the heated sample is sufficiently attenuated to allow the collection of a useful X-ray spectrum, but the filter member will absorb some X-ray photons, especially those of lower energy. To analyze an unheated sample, the filter cover 600 can be removed to restore the X-ray detector sensitivity to normal.

[0086] In some examples, a system is used in which the EDS detector is movable between two positions, for example, the filter member 700 is removably connected to a Figure 7 and Figure 8 A mounting element of a movable flap 710 is shown. The detector is closer to the sample in a first position than in a second position to achieve a high solid angle for collecting X-rays. This position is suitable for room temperature measurements. In the second position, the detector is retracted from the sample and behind a flap of material so that the filter assembly attenuates the radiation. An opening is provided in the flap to allow the detector's line of sight to the sample, and a filter assembly is mounted over the opening in the flap to reduce blackbody radiation from the sample while allowing transmission of X-rays. The filter material element of the filter assembly itself can be mounted in a cover, such as Figure 5 As shown, and the cover is installed on the opening. In the case where the detector is located behind the filter member, it is in a position suitable for in-situ heating experiments at high temperatures (>600℃), very high (>1000℃) and extremely high temperatures (>1500℃). The filter member mounted on the baffle is designed to block blackbody radiation while allowing the transmission of characteristic X-rays from the heated sample. In this configuration, the filter member can usually be positioned at a distance of less than 60mm from the sample. Therefore, by providing a removable filter member, the same detector can be used to collect useful X-ray spectra from samples heated to high temperatures with the addition of a filter, or the same detector can be used to collect X-ray spectra with good low-energy sensitivity from unheated samples without the addition of a filter.

[0087] An example of this embodiment is Figure 7 and Figure 8 710 changes position when the detector is moved. The detector sensor is in the end of the tube or on a support arm that can be moved on a mechanical slide to a first position where the sensor is located in a light-tight housing away from an opening facing the sample covered by the baffle 710 and can be moved to a second position on the slide, the first position being outside the housing and closer to the sample where the baffle does not restrict the transmission of X-rays from the sample to the detector.

[0088] Figure 7 The detector is shown in a second position, ready for in situ heating of the sample stage, wherein the detector is retracted behind a baffle assembly 710 having an opening covered by a filter film that is part of a filter material element that attenuates blackbody radiation, particularly visible light, while transmitting characteristic X-rays from the sample.

[0089] Figure 8The detector is shown in a first position because it will be used with an unheated sample and is therefore fully inserted out of the reach baffle assembly 710 and close to the specimen sample. In this position, no additional filter material is in place and therefore the X-ray detection efficiency is as high as possible.

[0090] In this exemplary embodiment, the shutter 710 is held closed against the light-tight housing by a spring mechanism when the detector is retracted from the sample, and is pushed out to avoid blocking the light path when the detector is inserted closer to the sample for analysis without heating. In addition to the spring, the shutter 710 can be supported by a hinge at the top and closed using gravity.

[0091] like Figure 7 and Figure 8 As shown, with the filter member 700 mounted on the baffle assembly mechanism 710, it is very convenient to switch the detector configuration between a first position, in which the detector is close to the sample and has no additional filter, which maximizes sensitivity to X-rays for analyzing unheated samples, and a second position, in which the detector is further away and has an additional filter, which sacrifices some sensitivity to lower energy X-rays while strongly attenuating black body radiation from the sample, and which is at a safe distance to allow the sample to be heated to very high temperatures, up to 1500°C or more, without damaging the filter or the detector. This movement can be manually or motorized.

[0092] In another embodiment, the baffle 710 can be implemented as a shutter mechanism that can be closed or opened anywhere the detector is positioned, rather than relying on inserting and retracting the detector tube to move the filter member into and out of the X-ray path from the sample to the detector.

[0093] The choice of filter material and thickness is important to provide adequate attenuation of blackbody radiation. Examples of filter materials considered are beryllium, silicon nitride with an aluminum coating, polymers (e.g. polyimide) with an aluminum coating, carbon or graphene. Torma et al. suggest that for solar-blind windows, the attenuation of optical radiation should be >10 11 , and for Fig. 9 The calculated light transmission of a 1000 nm thick carbon filter shown in indicates that this material should be solar blind. Fig.10The X-ray transmission curves of a 1000nm thick carbon window were compared to a commercial "solar blind" window in which the silicon nitride thickness was 150nm and the aluminum coating was 250nm thick. The 150nm silicon nitride film is not self-supporting and is typically supported on a silicon grid that is 15μm thick and covers about 20% of the active area. The 1000nm carbon film is self-supporting and does not require a grid support, so at higher energies, where the film is transparent to X-rays, the total transmission is about 20% greater than that of a silicon nitride filter of the same total area. The carbon filter has effective X-ray transmission (between 90% transmission and 30% transmission) below 280eV (down to 100eV), which can be used to detect X-rays from carbon and boron, while the silicon nitride filter has very little transmission for X-rays below 200eV and is insensitive to these elements. However, at energies between 300eV and 1100eV, the silicon nitride window has better transmission. In summary, both of these "solar blind" window materials provide similar levels of X-ray transmission, but there are some advantages other than X-ray transmission for the carbon-based windows.

[0094] exist Fig. 9 In the example, the calculated optical transmission of a 1000 nm thick carbon film is compared with the calculated optical transmission of a 250 nm thick aluminum layer. Fig.10 The silicon nitride windows used in the CMOS provide most of the optical attenuation. Carbon films provide increasing attenuation for shorter wavelength radiation, according to Figure 3 , this shorter wavelength radiation becomes more significant at very high sample temperatures.

[0095] In fact, carbon filters can be realized by multi-layer graphene, which makes the carbon filter stronger. In addition to providing a convenient self-supporting membrane for installation in Figure 5 In addition to the cover shown, the thick film is also more resilient than brittle silicon nitride films to small particle projectiles that can break freely from the heated sample and be projected toward the film by electrostatic or mechanical forces.

[0096] The thickness of a suitable carbon or graphene filter may typically be in the range of 100 nm to 1000 nm. A thickness of 1000 nm is more suitable for very high temperatures (>1500°C). A thickness of 100 nm to 300 nm may be sufficient for sample heating temperatures in the range of 600°C to 1000°C, and an aluminum coating may also be applied to the graphene filter to provide a different compromise between X-ray transmission and optical transmission, where this may be beneficial to the application.

[0097] In some examples, multi-layer coatings of different materials (eg, metal or inorganic films and organic polymer films) may form the filter material to provide different tradeoffs between X-ray transmission and optical transmission.

[0098] In addition to the examples provided above, the systems and methods described herein may also include the following features:

[0099] In some examples, a system for performing X-ray analysis of a sample in a particle beam instrument is provided, wherein the sample is located on a sample stage in a vacuum environment and the sample is heated to a temperature greater than 100°C; wherein, in a first mode, the analysis system includes a detector for the X-rays and an additional filter located between the sample and the detector, wherein the filter transmits the X-ray photons required for the analysis while providing sufficient attenuation of the blackbody radiation to avoid saturating the X-ray detector, and wherein the analysis system has a second mode in which the filter can be removed to improve the X-ray detection efficiency for analyzing unheated samples.

[0100] In some examples, the filter is mounted on / through an opening in a light-tight cover, and the cover is removably mounted over an entrance collimator of the detector.

[0101] In some examples, the filter is mounted on / through an opening in a baffle of light-opaque material, and in a first configuration, the detector entrance collimator is behind the opening in the baffle so that X-rays from the sample must pass through the filter to reach the detector, and in a second configuration, the baffle is moved to a position where there is no filter between the sample and the detector entrance collimator.

[0102] In some examples, the detector is located on a support arm that can be moved on a mechanical slide to a first position and can be moved to a second position on the slide, in which the detector is within a light-tight housing away from an opening facing the sample covered by a baffle, and the second position is outside the housing and closer to the sample, in which the baffle does not restrict the transmission of X-rays from the sample to the detector.

[0103] In some examples, the shutter is extended through the opening of the housing by a spring tension mechanism, or is supported on a hinge and held in place by gravity.

[0104] In some examples, a shutter mechanism can be used to move the baffle into and out of position between the sample and the detector.

[0105] In some examples, the filter is made of silicon nitride or a polymer or beryllium foil with a coating of at least 200 nm of aluminum.

[0106] In some examples, the filter is made of carbon or multi-layer graphene with a thickness between 100 nm and 1000 nm.

[0107] In some examples, the filter is held in place by friction and is free to expand and contract without inducing additional mechanical stress.

[0108] In some examples, the samples were heated to over 1000 degrees Celsius.

[0109] In some examples, the filter is positioned less than 60 mm from a portion of the sample.

[0110] In some examples, the particle beam is an electron beam.

[0111] In some examples, a filter member is provided that is adapted to be attached to a system for performing X-ray analysis of a sample in a particle beam instrument, the filter being removably attached to the system at a location between the sample and a detector of the system,

[0112] The filter is adapted to transmit the X-ray photons required for analysis while providing sufficient attenuation of black body radiation to avoid saturating the system's X-ray detectors.

[0113] In some examples, the filter assembly further includes a removable cover adapted to be mounted to an end of a detector housing of the system, the filter assembly being configured such that the filter is mountable to the removable cover.

[0114] In some examples, the filter component is configured to be secured to the system by an interference fit.

[0115] In some examples, the filter assembly includes a front cover, a spring element, a rear cover, and a threaded fitting for attaching the front cover to the rear cover, wherein the filter assembly is configured such that when the front cover and the rear cover are screwed together, the filter material can be held in place by friction against the spring element.

[0116] In some examples, the filter includes or is made of carbon or multilayer graphene, having a thickness between 100 nm and 1000 nm.

Claims

1. A system for performing energy dispersive X-ray analysis of a sample in a particle beam instrument, the system comprising an X-ray detector and a filter component, the system being adapted so that in a first operating mode, the filter component and the detector are positioned to provide an unobstructed line of sight between the sample and the detector, and in a second operating mode, the filter component and the detector are positioned to block the line of sight between the sample and the detector so that, in use, the proportion of blackbody radiation emitted from the sample that is incident on the detector is attenuated.

2. The system according to claim 1, wherein: In the first operating mode, all lines of sight between the active area of ​​the X-ray detector and the sample are unobstructed.

3. The system according to claim 1 or 2, wherein: In the second mode of operation, all lines of sight between the active area of ​​the X-ray detector and the sample are blocked.

4. A system according to any one of the preceding claims, wherein: The filter member is movable between a first position relative to the detector corresponding to the first mode of operation and a second position relative to the detector corresponding to the second mode of operation.

5. A system according to any one of the preceding claims, wherein: The detector is movable between a first position relative to the filter member corresponding to the first mode of operation and a second position relative to the filter member corresponding to the second mode of operation.

6. A system according to any one of the preceding claims, wherein: The system is adapted such that in the first operating mode, the detector is positioned closer to the sample than in the second operating mode.

7. A system according to any one of the preceding claims, wherein: The system includes a mounting element including an opening, and the filter member is removably attachable to the mounting element over the opening.

8. The system according to claim 7, wherein: The mounting element is movable between a first position relative to the detector corresponding to the first mode of operation and a second position relative to the detector corresponding to the second mode of operation.

9. The system according to claim 8, wherein: The mounting element is held in the second position by a spring tension mechanism, or supported on a hinge and held in position by gravity.

10. The system of claim 8 or 9, further comprising a motor, wherein: The motor is configured to actuate movement of the mounting element between the first position relative to the detector and the second position relative to the detector.

11. A system according to any one of claims 8 to 10, wherein: The X-ray detector is mounted to a support arm capable of moving along a mechanical slide between a first position relative to the filter component and a second position relative to the filter component, so that movement of the support arm toward the sample from the second position to the first position actuates the mounting element to move between the second position and the first position.

12. The system of any of the preceding claims, further comprising a shutter mechanism configured to move the filter member between a first position relative to the detector corresponding to the first operating mode and a second position relative to the detector corresponding to the second operating mode.

13. A system according to any one of the preceding claims, wherein: The filter member is configured to hold the filter material element in place by at least one of a friction fit, a clearance fit, and a transition fit.

14. A system according to any one of the preceding claims, wherein: The filter component further comprises a removable cover adapted to be mounted to the system, the filter component being configured such that a filter material element can be removably mounted to the removable cover.

15. A system according to any one of the preceding claims, wherein: The filter member comprises a resilient element adapted such that, in use, the resilient element exerts a force on the filter material element such that the filter material is held in position.

16. A system according to any one of the preceding claims, wherein: The filter member comprises a slot adapted to receive a filter material element such that the filter material element forms a clearance fit with the filter member.

17. A system according to any one of claims 13 to 16, wherein: The filter component comprises a front cover part, a spring element, a rear cover part and a threaded fitting for attaching the front cover part to the rear cover part, wherein the filter component is configured so that when the front cover part and the rear cover part are screwed together, the filter material element can be held in place by friction against the spring element.

18. A system according to any one of the preceding claims, wherein: The filter structure also includes a magnetic electron trap.

19. The system of claim 18, wherein: The filter member is adapted to enable an element of filter material to be inserted into the space between the electron trap and the detector.

20. A system according to any one of the preceding claims, wherein: An average thickness of a filter material included in the filter member along a direction between the sample and the detector is greater than or equal to 100 nm.

21. A system according to any one of the preceding claims, wherein: The filter member includes any one or more of silicon nitride, polymer, aluminum, beryllium, carbon or graphene.

22. A system according to any one of the preceding claims, wherein: The filter member comprises silicon nitride or a polymer with an aluminium coating of at least 200 nm, or a beryllium foil.

23. A system according to any one of claims 1 to 21, wherein: The filter member comprises carbon or multilayer graphene and has an average thickness between 100 nm and 1000 nm along a direction between the sample and the detector.

24. A method for performing energy dispersive X-ray analysis on a sample based on the first operating mode of the system according to any one of claims 1 to 23, the method comprising: positioning a sample on a sample stage within a sample chamber of the system; generating a focused particle beam using a particle beam assembly; as well as The energy of X-ray photons generated by the interaction between the particle beam and the sample is monitored using the X-ray detector.

25. A method for performing energy dispersive X-ray analysis on a sample based on the second operation mode of the system according to any one of claims 1 to 23, the method comprising: positioning a sample on a sample stage within a sample chamber of the system; heating the sample to a temperature greater than or equal to 100° C.; generating a focused particle beam using a particle beam assembly; as well as The energy of X-ray photons generated by the interaction between the particle beam and the sample is monitored using the X-ray detector.

26. The method according to claim 25, wherein: Heating the sample to a temperature greater than or equal to 100°C further includes heating the sample to a temperature greater than or equal to 600°C.

27. The method according to claim 25, wherein: Heating the sample to a temperature greater than or equal to 100°C further includes heating the sample to a temperature greater than or equal to 1500°C.

28. A method according to any one of claims 25 to 27, wherein: Monitoring the energy of X-ray photons generated by the interaction between the particle beam and the sample using the X-ray detector also includes positioning the filter member less than 60 mm from a portion of the sample.

Images