X-ray scattering equipment

Abstract

The present invention relates to an X-ray scattering device (10), which comprises: - a sample holder (16) for aligning and / or orienting a sample (17) to be analyzed by X-ray scattering; - a first X-ray beam delivery system (12), which comprises a first X-ray source (18) and a first monochromator (20) and is arranged upstream of the sample holder (16) for generating and guiding a first X-ray beam (22) along a beam path in the propagation direction (Y) towards the sample holder (16); - a distal X-ray detector (14), which is arranged downstream of the sample holder (16) and is movable, in particular in a motorized manner, along the propagation direction (Y) so as to detect the first X-ray beam (22) and X-rays scattered from the sample (17) at different scattering angles; - wherein the first X-ray beam delivery system (12) is configured to focus the first X-ray beam (22) onto a focal spot on or near the distal X-ray detector (14) when placed at a maximum distance from the sample holder (16), or to produce a parallel beam, characterized in that the X-ray scattering device (10) further comprises a second X-ray beam delivery system (55), which comprises a second X-ray source (551) and is configured to generate and guide a divergent second X-ray beam (58) towards the sample holder (16) for X-ray imaging. The present invention also relates to an X-ray scattering method using such an X-ray scattering device.

Description

Technical Field

[0001] The present invention relates to X-ray scattering equipment. Background Art

[0002] Generally, X-ray scattering and X-ray diffraction instruments include:

[0003] 1) A source

[0004] 2) A wavelength selector (monochromator)

[0005] 3) A collimation section (defining the beam direction and removing residual background scattering or divergence)

[0006] 4) A sample area

[0007] 5) And a detector area.

[0008] In the years following X-ray analysis, due to the need for faster measurements and better data quality, great developments have been made in each component, thus providing characterization answers for an increasing number of structured and quasi-structured sample groups.

[0009] In addition, various highly specialized diffraction and scattering geometries have been developed to extract more specific information, such as:

[0010] 1) X-ray powder diffraction

[0011] a. Bragg-Brentano reflection

[0012] b. Guinier transmission

[0013] 2) Single crystal diffraction (transmission)

[0014] 3) Back-reflection Laue

[0015] 4) Grazing incidence X-ray diffraction

[0016] 5) X-ray reflectivity

[0017] 6) Texture

[0018] 7) Small angle X-ray scattering (transmission)

[0019] 8) Wide angle X-ray scattering (transmission)

[0020] 9) Bonse-Hart ultra-intelligent angle scattering

[0021] To maximize the instrument investment, several X-ray scattering devices allow for easy switching between different configurations. For example, one can mention switching the wavelength by changing the source anode material, such as the Xenocs Dual-Source SAXS, or one can mention the technique of switching by changing the collimation components. Thus, with only a small additional cost, the instrument can be re-optimized for entirely new scattering or diffraction applications.

[0022] Materials science and development require structural characterization at large length scales to study the impact of hierarchical structures on material functions. Complex materials exhibit more or less structured entities depending on the length scale. In addition, the development of new materials will require in-situ characterization based on external parameters or structural characterization during operation. By analyzing the intensity of the X-ray beam elastically scattered by the sample, nanostructured materials with structures typically having a length scale of 1 nm to 150 nm can be characterized by small-angle X-ray scattering (SAXS) in a scattering angle range typically from 0.05° to 10° when the two phases have sufficient electron density contrast. This technique has been widely used for soft matter characterization, such as in the fields of polymers, colloids, or proteins in solution.

[0023] New material characterization requires the combination of wide-angle X-ray scattering (WAXS) to characterize the crystal structure, and most SAXS characterization instruments combine SAXS / WAXS and USAXS (ultra-small angle X-ray scattering) to probe structures on the order of up to a few micrometers, such as using the USAXS Bonse-Hart configuration to measure only the scattering profile in one direction.

[0024] In other words, while wide-angle X-ray scattering (WAXS) can generally obtain information related to the crystallinity and crystal phase of the sample to be analyzed, small-angle X-ray scattering (SAXS) can generally obtain information related to the sample structure (nanostructure) at the nanoscale. Since both the crystal phase and the nanostructure affect material properties, there is interest in performing SAXS and WAXS simultaneously on the same sample and the same instrument.

[0025] However, although most of the X-ray techniques mentioned above can be optimally configured in a fairly compact apparatus suitable for desktop applications, or at most a smaller laboratory apparatus with a footprint less than 2 m by 2 m, this is not the case for SAXS apparatuses, where long instruments (3 m to 10 m) always provide a better combination of resolution and intensity. Shorter instruments provide lower intensity at the highest resolution required in SAXS, so the apparatus remains longer.

[0026] Nonetheless, recent developments have started to combine conventional SAXS with other configurations, such as Bonse-Hart ultra-small angle X-ray scattering, grazing incidence diffraction, wide-angle X-ray scattering, and powder and texture analysis.

[0027] For SAXS and WAXS measurements on the same sample and instrument, an X-ray scattering device can be purchased from the present applicant under the name "Xeuss 3.0", which comprises:

[0028] - A sample holder for aligning and / or orienting a sample to be analyzed by X-ray scattering;

[0029] - A first X-ray beam delivery system, which includes a first X-ray source and a first monochromator and is arranged upstream of the sample holder for generating and guiding a first X-ray beam along a beam path in the propagation direction towards the sample holder;

[0030] - A distal X-ray detector, which is arranged downstream of the sample holder and is movable, in particular motorized, along the propagation direction so as to detect the first X-ray beam and X-rays scattered from the sample at different scattering angles;

[0031] wherein the first X-ray beam delivery system is configured to focus the first X-ray beam onto a focal spot on or near the distal X-ray detector when placed at the maximum distance from the sample holder, or is configured to produce a parallel beam.

[0032] The first X-ray beam delivery system of such a conventional X-ray scattering device includes a first X-ray source for generating X-rays, such as a source with a Cu or Mo anode, and an optical and collimation system including a first monochromator for guiding and conditioning the generated first X-ray beam along a substantially horizontal propagation direction towards the sample holder, which may include motorized translation and / or rotation stages and other typical sample stage devices known in the field of X-ray scattering and which can be placed in a vacuum chamber.

[0033] Such a conventional X-ray scattering device includes at least one X-ray detector, which is arranged downstream of the sample holder, i.e., on the side of the sample holder opposite to the side where the first X-ray beam delivery system is located:

[0034] A far - side X - ray detector is typically mounted on a detector stage that allows translation along the propagation direction of the direct beam at a large horizontal distance from the sample holder - typically in the range of 50 mm to 1000 mm or more, e.g., up to 5000 mm. Depending on the position details of the far - side X - ray detector and the size of its sensors, the far - side X - ray detector is typically able to detect X - rays scattered from the sample, where the scattering angle of these X - rays relative to the direct X - ray beam ranges from as small as approximately 2θ = 0.05° to as large as 60° to 70°. Thus, the far - side X - ray detector is suitable for small - angle X - ray scattering (SAXS) that provides information related to the sample structure at the nanoscale level and wide - angle X - ray scattering (WAXS) that provides information related to the sample crystallinity.

[0035] Scientists have developed new materials - such as plastics, elastomers, composites, foams, textiles, biopolymers - for combining X - ray scattering measurements with X - ray imaging, particularly absorption - or phase - contrast - based X - ray radiography, which is particularly advantageous for light - element materials (or materials with low Z). Some example applications of combining these techniques are the characterization of semi - crystalline polymers, polymer fibers, or nanocomposites, where atomic - scale and nanoscale structural information and their orientation can be combined with X - ray imaging information to optimize mechanical properties or other material characteristics. For polymer materials, examples of relevant parameters are the crystallinity and microcrystalline orientation determined using WAXS, the nanoscale domain size and its orientation determined using SAXS, while voids and cracks in the material can be measured using X - ray radiography. Studying the correlations of these parameters may be highly relevant to the development of new materials. Thus, if all the techniques are combined, two different instruments or even more must be used, which limits the systematic use of combined analysis methods.

[0036] Furthermore, cross - comparison of the measurements can be tricky and takes time to set up all the experiments because, on the one hand, the field of view for imaging is different, and on the other hand, the SAXS / WAXS characterization is different (which may require cutting the sample or pre - positioning the analysis area for further X - ray scattering experiments). One advantage of the present invention is to combine the measurement techniques of X - ray scattering (SAXS and WAXS) and X - ray imaging (absorption and / or phase - contrast radiography) on the same device so as to be able to systematically analyze the same sample using both techniques. The device can be advantageously used, for example, in in - situ dynamic experiments (where the sample is exposed to temperature, stress, shear, humidity, or other types of external actions), by sequentially using the X - ray scattering and X - ray imaging measurement channels during the in - situ dynamic experiment to provide information over a wider length scale.

[0037] In addition, another advantage would be the improvement of X-ray scattering analysis of large samples of a few millimeters in size with inhomogeneous properties, which may require prior mapping of the sample, since the typical X-ray footprint on a SAXS / WAXS instrument is usually in the range of less than 1 mm2. This task is typically accomplished by performing an X-ray transmission map (or absorption map) of the sample, thereby measuring the transmission intensity of the direct X-ray beam passing through the sample in order to define the region of interest for further SAXS or WAXS characterization. This absorption mapping contrast requires very long measurement times using an X-ray scattering analysis device, since the X-ray beam delivery system provides a monochromatic beam with a controlled divergence and beam size on the sample required for SAXS. Another advantage of the present invention is to provide an improved X-ray scattering device having optimal conditions for performing SAXS / WAXS experiments on large inhomogeneous samples (inhomogeneities on the order of a few hundred microns to millimeters). SUMMARY OF THE INVENTION

[0038] Accordingly, it is an object of the present invention to provide an improved X-ray scattering device of the above type which allows optimal conditions to be provided for SAXS and X-ray imaging measurements, respectively.

[0039] According to the present invention, this object is achieved by an X-ray scattering device of the above conventional type, characterized in that the X-ray scattering device further comprises a second X-ray beam delivery system which includes a second X-ray source and is configured to generate and direct a divergent second X-ray beam towards the sample holder for X-ray imaging.

[0040] Since the second X-ray beam delivery system for imaging is provided as part of the same X-ray scattering device, there is no longer a need to move the sample between different instruments. In addition, the second X-ray source generates and directs a divergent second X-ray beam towards the sample holder, which has beam characteristics optimized for X-ray imaging. Therefore, there is no need to also use the first X-ray beam, which is typically optimized for SAXS or WAXS measurements, for imaging purposes, thus saving valuable measurement time. The X-ray scattering device according to the present invention particularly allows X-ray imaging analysis of a sample mounted on the sample holder using the second X-ray beam, then defining a region of interest in or on the sample based on the results of the X-ray imaging analysis, and continuously performing X-ray scattering analysis of the region of interest using the first X-ray beam, for example, by SAXS and / or WAXS measurements.

[0041] In one embodiment of the X-ray scattering device according to the present invention, the angle of the propagation direction of the second X-ray beam relative to the propagation direction of the first X-ray beam is less than or equal to 10°. In particular, the second X-ray beam may be parallel to the first X-ray beam. Since the two X-ray beams then propagate parallelly or almost parallelly, the far-side X-ray detector can be used not only for SAXS / WAXS measurements carried out in the usual way, but also for X-ray imaging measurements. For this purpose, the far-side X-ray detector can be moved not only along the propagation direction of the first X-ray beam, but also in a plane perpendicular to the propagation direction of the first X-ray beam.

[0042] In one embodiment of the embodiments of the present invention, the second X-ray beam delivery system may be fixedly located at a position upstream of the sample holder to allow the first X-ray beam to pass through. This allows the two X-ray beams to reach the sample environment, such as the vacuum chamber where the sample holder is located. If the sample is large enough and the source is very compact, in principle both beams can reach without moving.

[0043] However, in these embodiments of the X-ray scattering device according to the present invention having parallel or almost parallel X-ray beams, preferably, the sample holder can be moved in a plane perpendicular to the propagation direction of the first X-ray beam, particularly in a motorized manner. This allows the sample to be moved from a first measurement position in which it intercepts the first X-ray beam for SAXS and / or WAXS measurements to a second measurement position in which it intercepts the second X-ray beam for imaging measurements, and vice versa.

[0044] Instead of fixedly locating the second X-ray beam delivery system at a position upstream of the sample holder to allow the first X-ray beam to pass through, the X-ray scattering device according to the present invention may further include an insertion module configured to move the second X-ray beam delivery system into the first X-ray beam at a position upstream of the sample holder. The insertion module may allow computer-controlled movement of the second X-ray beam delivery system, thus avoiding any manual interaction by the user.

[0045] In this case, the X-ray scattering device preferably further includes a main collimator extending along the beam path from a position downstream of the first X-ray beam delivery system to a position upstream of the sample holder, wherein the insertion module includes a motorized platform configured to alternatively position the second X-ray beam delivery system or the collimator extension into the beam path at a position between the main collimator and the sample holder. For SAXS measurements, the collimator extension is then positioned in the beam path, allowing the first X-ray beam to irradiate the sample mounted on the sample holder as a direct beam. However, for imaging measurements, the second X-ray beam delivery system is positioned in the beam path by the motorized platform. The computer control system of the X-ray scattering device can then enable the shutter of the first X-ray beam delivery system to block the first X-ray beam, while enabling the shutter of the second X-ray beam delivery system to cause the second X-ray beam to irradiate the sample mounted on the sample holder.

[0046] Preferably, the downstream end of the main collimator and the upstream end of the collimator extension are respectively provided with connection elements for vacuum-tight connection. This allows the beam path to be substantially maintained in a vacuum from the first X-ray beam delivery system to the sample holder during SAXS measurements when the collimator extension is positioned in the beam path.

[0047] Instead of using parallel or nearly parallel first and second X-ray beams so as to use a far-side X-ray detector for SAXS / WAXS and for imaging measurements, other embodiments of the X-ray scattering device according to the present invention are characterized in that the angle of the propagation direction of the second X-ray beam relative to the propagation direction of the first X-ray beam is greater than 10°. In these embodiments, the second X-ray beam delivery system is preferably located at a position upstream of the sample holder to allow the first X-ray beam to pass through, and further includes a near-side X-ray detector arranged downstream of the sample holder to allow the first X-ray beam to pass through and to detect the X-rays transmitted through the sample from the second X-ray beam delivery system. This near-side X-ray detector can be used not only for the imaging measurements according to the present invention, but also for WAXS measurements, as described in detail in the applicant's European patent application 19290126.2, the content of which is incorporated herein by reference.

[0048] In a preferred further development of this embodiment, the sample holder and / or the proximal X-ray detector can be rotated about at least one axis of rotation passing through the sample holder and perpendicular to the propagation direction of the second X-ray beam, in particular in a motorized manner. This allows the sample to be rotated from a first measurement position, in which it intercepts a first X-ray beam for SAXS and / or WAXS measurements, to a second measurement position, in which it intercepts a second X-ray beam for imaging measurements, and vice versa, where in both measurement positions the sample surface is substantially perpendicular to the respective X-ray beam.

[0049] Preferably, the X-ray scattering device according to the invention further comprises an object insertion unit adapted to insert a randomly structured object into the second X-ray beam upstream or downstream of the sample holder. This allows a special type of X-ray phase contrast imaging analysis based on the measurement of the refraction angle, and a phase contrast map is obtained by comparing the patterns generated by the randomly structured object when placed in the beam with and without sample interaction. Speckle-based phase contrast imaging is one of these methods described in detail in combination with the method according to the invention.

[0050] Alternatively, the X-ray scattering device according to the invention comprises an object insertion unit adapted to insert a structured object with a repeating structure into the second X-ray beam, the structured object being adapted to produce a wavefront modulation of the second X-ray beam, so as to obtain a phase map of the sample by comparing the images generated by the structured object when placed in the beam with and without sample interaction.

[0051] Preferably, the X-ray scattering device according to the invention further comprises a mask insertion unit adapted to insert a diffraction mask into the second X-ray beam upstream or downstream of the sample holder, the diffraction mask being adapted to produce a modulation pattern of the X-ray beam, so as to produce a two-dimensional dark field image of the sample by comparing the patterns generated by the diffraction mask when placed in the beam with and without sample interaction.

[0052] In all embodiments and further developments, the X-ray scattering device according to the invention preferably further comprises a computer control system configured to control the X-ray scattering device so as to perform measurements one after another or simultaneously using the first X-ray beam delivery system and the second X-ray beam delivery system.

[0053] The invention also relates to an X-ray scattering method using the X-ray scattering device as described above, which X-ray scattering method preferably comprises the following steps:

[0054] - Performing X-ray imaging analysis on a sample mounted on a sample holder using the second X-ray beam;

[0055] - Defining a region of interest in or on the sample based on the result of the X-ray imaging analysis; and

[0056] - Performing X-ray scattering analysis on the region of interest using the first X-ray beam.

[0057] The X-ray imaging analysis of the sample may include various imaging methods to be described below:

[0058] Phase-contrast imaging

[0059] The described X-ray scattering device according to the present invention allows the performance of the method according to the present invention, thereby obtaining an X-ray image based on the sample absorption contrast with a resolution of several micrometers to several tens of micrometers. In a preferred embodiment of the present invention, the X-ray imaging component of the device is also suitable for phase-contrast imaging in order to perform X-ray imaging on samples with low absorption contrast. X-ray imaging is based on the contrast of X-ray attenuation when passing through a medium. The attenuation and phase contrast are basically determined by β and δ respectively, which are the imaginary and real parts of the complex refractive index n of the material (n = 1 - δ + iβ). In the hard X-ray region (for high energies), δ of low-Z materials is much larger than β. For light materials, especially when using higher energies (>10 keV), phase-contrast imaging is more sensitive than absorption-contrast imaging.

[0060] Since the device of the present invention is a combined X-ray scattering and X-ray imaging system, the materials to be used are generally low-Z materials that do not require an X-ray source for high-energy imaging. The phase-contrast imaging channel is still very beneficial for edge enhancement or imaging features with an absorption contrast close to that of the matrix.

[0061] Different X-ray phase-contrast imaging methods can be used. Some methods are based on measuring the refraction angle caused by phase contrast, and some other methods are based on interferometric methods.

[0062] Propagation-based phase-contrast imaging

[0063] In an embodiment of the present invention, phase-contrast imaging is achieved using a second beam delivery system without any additional components by analyzing the free propagation of an X-ray wavefront and studying the effect of the sample on such a wavefront. By using an increased propagation distance (i.e., increasing the distance between the object and the detector), the imaging progresses from absorption-contrast images to the near-field imaging regime, where phase changes develop into intensity changes that can be detected. Phase-contrast imaging using the propagation-based method (PBI) requires an X-ray source with high spatial coherence. The PBI method is used together with an X-ray imaging source having a spot size smaller than 50 microns, preferably smaller than 10 microns, and an X-ray imaging source generating a primary energy (the fluorescent line of the anode being between 8 keV and 30 keV), such that the propagation distance remains in the near field.

[0064] Since phase contrast becomes more pronounced as the effective propagation distance is extended, the use of the PBI phase-contrast imaging channel according to the present invention may include: measuring an X-ray image of the sample using absorption contrast with a large field of view on the sample, using a small object-to-detector distance S1', determining potential regions of interest (i.e., regions where specific features are suspected or expected), and based on this image, measuring a second image at a longer distance S1' using phase-contrast imaging for better feature enhancement. For example, phase-contrast imaging can be used to define a welding zone in case the bonding material has equivalent absorption contrast, to define the proper positioning of small-angle X-ray scattering measurement locations.

[0065] In another embodiment of the method according to the present invention, X-ray scattering analysis of the sample can be performed first. Based on the results and the potential uncertainties of the sample, X-ray phase-contrast imaging can be performed to verify such uncertainties (the presence of aggregation states at the SAXS measurement location or in different entities), which would not be detected due to the potential lack of contrast in the X-ray absorption image.

[0066] Phase-contrast imaging data processing includes a phase retrieval process to extract phase information from absorption information. In a preferred embodiment, the data algorithm used is adapted to separate and extract this information based on a single propagation distance (a single detector measurement location) - in another embodiment of the present invention, an algorithm using multiple acquisition distances is used.

[0067] Phase-contrast imaging with phase modulation structure

[0068] In another embodiment of the present invention, phase-contrast imaging can be accomplished by generating a phase image created by a structured object having a repetitive structure, which is adapted to produce a wavefront modulation of a second X-ray beam and a phase map of a sample by comparing images generated by the structured object when placed in the beam with and without sample interaction. The structured object can be an absorbing structure made of a periodic array of absorbing structures or a phase grating, such as a Hartmann mask.

[0069] In the case of a Hartmann mask, the incident beam is modulated by the absorbing structure into a parallel beam, and the sample phase map is reconstructed by analyzing the deflections produced by the sample. One of the advantages of this method is that it limits the number of inserted objects between the sample and the detector, since the period of the absorbing structure can be made large enough compared to the wavelength to enable direct reconstruction of the phase pattern on the detector.

[0070] In the case where the structured object is a phase grating, the incident X-ray beam is phase-modulated and an interference fringe pattern is produced at a specific distance (Talbot distance). This interferometric method generally requires a monochromatic highly coherent source and precise positioning of the grating. In practice, other gratings (absorbing) may be needed on the source side to increase the coherence of the source or near the detector to increase the detector resolution.

[0071] In a preferred embodiment of the present invention, an X-ray phase-contrast imaging method is sought, in which a limited number of components must be implemented in the displacement path of the far detector, as is the case for the Talbot interferometric method. For operation in the SAXS measurement mode, the system allows the far detector to move along the beam propagation direction, so methods with limited implementation complexity can be considered.

[0072] In another embodiment of the present invention, phase-contrast imaging is used based on comparing images generated by a reference object when placed in the beam with and without sample interaction, and the reference object is a random structured object. This method is generally referred to as speckle-based phase-contrast imaging.

[0073] Speckle-based phase-contrast imaging is particularly advantageous because it does not require a very high spatial coherence of the source (a source greater than 10 microns can be used), and the manufacturing cost of the random structured object is moderate compared to the phase gratings used in Talbot X-ray interferometric methods.

[0074] Speckle-based phase-contrast imaging

[0075] In this embodiment of the invention, the use of the second X-ray beam delivery system is combined with the insertion of a random structure object, preferably in front of the sample holder, for speckle-based phase contrast imaging as described above in connection with the object insertion unit.

[0076] The imaging characterization steps generally include: measuring the speckle pattern generated by the random structure object on the distal detector placed at a distance without any sample in place to interact with the propagating second X-ray beam, and performing an additional exposure with the sample and the random structure object in place to record the distorted image of the speckle pattern caused by the sample on the distal detector at the same distance. By performing a correlation analysis on the speckle patterns with and without the sample, a two-dimensional phase map of the sample can be retrieved, where the resolution depends on the size of the speckles, i.e., the resolution of the features of the random structure object, and the size of the pixels of the distal detector and its distance from the sample. The random structure object is a sample made of a random structure with small features and high X-ray intensity contrast, such as sandpaper or cardboard. This alternative characterization sequence for speckle X-ray imaging can include scanning the speckle patterns at different lateral positions of the random structure object, where the step size of the movement is less than the speckle size to increase the spatial resolution.

[0077] X-ray speckle imaging is a particularly advantageous phase contrast imaging method because it does not require a complex grating structure and reduces the requirements for the spatial coherence of the source to be used.

[0078] In speckle-based imaging, when the X-ray irradiates the diffuser, i.e., the random structure object, a speckle pattern is generated on the detector plane. When a sample with absorption, scattering, or phase shift characteristics is placed in the beam, the global intensity (due to the absorption contrast A, A = (1 - T), where T is the transmittance), position (displacement δ caused by the refraction angle related to the phase of the sample), and amplitude (due to small-angle X-ray scattering: the intensity scattered by the sample blurs the speckle pattern, resulting in a reduction in the contrast D after sample transmission correction) of the speckle reference pattern change. Measuring the line profile of the X-ray intensity at the detector plane allows the extraction of the parameters T, δ, D from the two-dimensional image of the modified speckle pattern at the detector. Through a reconstruction algorithm, therefore, speckle-based imaging can be used to obtain multiple two-dimensional X-ray images corresponding to the absorption contrast, phase contrast, and dark-field contrast (due to the scattering regions in the sample), respectively. In speckle-based imaging, the phase contrast image is obtained by analyzing the displacement δ of the speckle pattern along the horizontal and vertical directions. This can typically be done by analyzing the displacement in a single exposure using a window analysis of several pixels. This analysis window limits the resolution of speckle-based phase contrast imaging to its corresponding size. As described above, compared to the single-exposure method, alternative analysis methods will use multiple exposures with the random structure object at different positions to improve the resolution.

[0079] Dark-field imaging

[0080] In a preferred embodiment of the present invention, the X-ray imaging channel is also capable of performing dark-field imaging. Advantageously, this image can be obtained together with absorption and phase-contrast imaging, just as in speckle-based imaging. Interferometric methods can also be used, as they provide absorption, phase-contrast, and dark-field imaging. In this case, a motorized insertion device is provided in the device according to the invention to insert a phase grating and potentially a detector grating. In the case of a one-dimensional grating, the grating insertion device can include rotating the grating 90° towards the detector to perform two consecutive experiments and obtain a two-dimensional dark-field image. These insertion devices need to be synchronized with the SAXS measurement channel so that the detector can be freely moved to change the resolution in the SAXS / WAXS measurement.

[0081] As an alternative to dark-field imaging using a one-dimensional grating in X-ray interferometric methods, a two-dimensional diffraction structure can be used to directly perform two-dimensional imaging. In this embodiment, the X-ray scattering device according to the invention includes a mask insertion unit adapted to insert a diffraction mask into the second X-ray beam downstream of the sample holder, the diffraction mask being adapted to generate a modulated pattern of the X-ray beam in order to generate a two-dimensional dark-field image of the sample by comparing the patterns generated by the diffraction mask with and without sample interaction. For example, the two-dimensional diffraction mask can include concentric absorption rings arranged with a predetermined first period, each absorption ring being made of an absorption structure including additional concentric rings arranged with a predetermined second period smaller than the first period, so as to be adapted to generate a modulated pattern of the incident beam. By analyzing the local reduction in the visibility of the X-ray pattern generated by the diffraction mask when the sample is inserted, a two-dimensional dark-field image can be created. The local reduction in the visibility of the X-ray pattern is caused by small-angle X-ray scattering of the structures inside the sample.

[0082] The embodiments of the present invention using dark-field imaging are particularly advantageous because they can combine large-field-of-view imaging measurements in the dark field to identify scattering regions (isotropic or anisotropic), or regions with increased scattering and quantitatively analyze these regions with the SAXS measurement channel. In fact, although dark-field imaging will identify the scattering regions, the angular dependence of this scattering signal will not be obtainable or additional measurements (at different distances) will be required to identify the scattering signals from different real-space correlations.

[0083] In an X-ray scattering measurement channel, a two-dimensional X-ray scattering intensity image is collected on a detector and the angular correlation (i.e., wave vector) is retrieved by azimuthal averaging, thereby providing additional quantitative information on all characteristic dimensions contributing to the scattering signal in real space. In addition, the dark-field imaging intensity is strongly influenced by the scattering intensity from the largest characteristic size (micrometer-scale size), which can be measured using a USAXS measurement channel or a SAXS measurement channel at a large sample-to-detector distance.

[0084] Thus, in a preferred embodiment of the method according to the invention, the X-ray imaging analysis includes combined absorption, phase-contrast, and dark-field imaging measurements, and the X-ray scattering analysis includes USAXS measurement and / or SAXS measurement and / or WAXS measurement.

[0085] Preferably, the phase-contrast imaging step includes acquiring images of the sample at different sample-to-detector distances, which includes at least one measurement step with a shorter field of view (i.e., a larger sample-to-detector distance), centered at a predefined sample position based on absorption and phase imaging measurements with a larger field of view, for better phase contrast and feature definition.

[0086] The method according to the invention may further include simultaneous or additional dark-field image acquisition to define regions of interest with different scattering intensities compared to other regions and using a USAXS measurement channel or a SAXS measurement channel to define regions of interest for further X-ray scattering analysis of the sample to obtain quantitative information related to the characteristic dimensions contributing to the dark-field signal and / or to identify additional characteristic dimensions with smaller dimensions.

[0087] In this case, the X-ray scattering method according to the invention may include acquiring additional dark-field signal images under different measurement settings to detect additional scattering signal contributions from other characteristic dimensions, wherein the characteristic dimensions to be detected have been determined by previous USAXS and SAXS measurements. Description of the Drawings

[0088] Preferred embodiments of an X-ray scattering device according to the invention will be described below with reference to the drawings, in which:

[0089] Figure 1a A first embodiment of an X-ray scattering device according to the invention is shown, in which a first X-ray beam delivery system and a second X-ray beam delivery system are arranged adjacent to each other in a configuration for SAXS measurement;

[0090] Figure 1b The embodiment of Figure 1a in a configuration for X-ray imaging measurement is shown;

[0091] Figure 2 Shows a second embodiment of an X-ray scattering device according to the present invention, the X-ray scattering device including an insertion module for moving a second X-ray beam delivery system into a first X-ray beam;

[0092] Figure 3 Shows a third embodiment of an X-ray scattering device according to the present invention, wherein the propagation direction of the second X-ray beam intersects the propagation direction of the first X-ray beam at the sample position;

[0093] Figure 4 Shows according to Figure 2 A modification of the second embodiment, wherein an additional object insertion unit is provided in the vacuum chamber for accommodating the sample: and

[0094] Figure 5 Shows a modification of the second embodiment according to Figure 4 Equipped with an additional X-ray beam delivery system for WAXS measurement. Detailed embodiments

[0095] Figure 1a Shows a schematic top view of a first embodiment of an X-ray scattering device 10 according to the present invention, the X-ray scattering device 10 being in a configuration for SAXS measurement, also referred to as the "SAXS channel". The device 10 is shown from its upstream end at the first X-ray beam delivery system 12 down to its downstream end at the distal X-ray detector 14. The device 10 is used to analyze a sample mounted on a sample holder 16.

[0096] In all top views shown in the figure, the upstream end of the X-ray scattering device 10 is on the left and the downstream end is on the right. Therefore, the propagation directions Y of the first X-ray beam and the second X-ray beam are from left to right.

[0097] Furthermore, it is assumed that the propagation direction Y is horizontal in the laboratory system. In all figures, the horizontal direction perpendicular to Y is referred to as the X direction, and the vertical direction perpendicular to X and Y is referred to as the Z direction pointing out of the plane of the paper.

[0098] The first X-ray beam delivery system 12 includes a first X-ray source 18 and a first monochromator 20. As Figure 1aAs shown by the dashed line in, the first monochromator 20 is selected and set to collect, for example, X-rays generated by the first X-ray source 18 and to focus the X-rays as a first X-ray beam 22 onto the distal X-ray detector 14 or onto a focal spot near the distal X-ray detector 14 when the distal X-ray detector 14 is arranged at a maximum distance from the sample holder 16 in the Y direction. Herein, "near" means that the distance between the focal spot of the first X-ray beam 22 and the distal X-ray detector 14 is approximately 20% of the distance P2 (indicated by the double arrow in Figure 1a ) between the focal spot and the first monochromator 20. The focal spot can be before (i.e., upstream) or after (i.e., downstream) the distal X-ray detector 14. Alternatively, the first monochromator 20 can also produce a substantially parallel beam.

[0099] The first X-ray source 18 is preferably a point-focusing source, and the first monochromator 20 is preferably a point-focusing monochromator.

[0100] The beam shape can be further defined by a slit module 24, preferably of the "scatter-free" or "scatter-suppressed" type. In Figure 1a , two such slit modules 24 are shown, a first slit module immediately downstream of the first monochromator 20 and a second slit module immediately upstream of the vacuum chamber 26. The vacuum chamber 26 houses the sample holder 16, which can include a motorized translation and / or rotation stage and other typical sample stage devices known in the field of X-ray scattering.

[0101] For WAXS experiments, the distal X-ray detector 14 can be moved along the propagation direction Y towards the vacuum chamber 26, particularly in a motorized manner. However, in the Figure 1a embodiment shown, the proximal X-ray detector 44 is located inside the vacuum chamber 26 and allows the detection of the WAXS signal scattered or diffracted from the sample.

[0102] The X-ray scattering device 10 further includes a second X-ray beam delivery system 55, which includes a second X-ray source 551 and is configured to generate a divergent second X-ray beam and direct the second X-ray beam towards the sample holder 16 for X-ray imaging. Although the second X-ray beam delivery system 55 is inactive in the Figure 1a SAXS configuration shown in, the second X-ray beam delivery system 55 is active in the Figure 1b imaging configuration - also referred to as the "imaging channel" - shown in and is described below:

[0103] The second X-ray beam delivery system 55 is configured to produce a conical beam 58 that propagates towards the distal X-ray detector 14. The conical beam 58 is in Figure 1bis indicated by the dashed line. The second X-ray source 551 is preferably a source with a solid anode - such as chromium, copper, molybdenum, silver, or tungsten - and emits an X-ray beam with a wide energy distribution, i.e., including the characteristic fluorescent lines (Kα, Kβ, Lα) of the anode and bremsstrahlung. In a preferred embodiment of the present invention, the second X-ray beam delivery system 55 produces a polychromatic beam that has a much lower monochromaticity compared to the first X-ray beam 22 for SAXS. Most of the X-ray beam 58 still consists of the characteristic fluorescent lines of the anode. The second X-ray beam delivery system 55 also includes a light valve coupled to the main slit module 56 to define a conical beam for irradiating a sample area within a few millimeters. The second X-ray beam delivery system 55 may also include a filter. And the slit module 56 may be a combination of slits to control the size of the conical beam 58, where a cone within a range of a few degrees is typically used. The second X-ray source 551 can generally be a source with a tungsten or molybdenum anode excited up to 50 kV, alternatively up to 70 kV, depending on the material to be analyzed and the small focal size, i.e., a focal point of 50 microns or less, preferably 10 microns or less.

[0104] In Figure 1a and Figure 1b the embodiment shown, the second X-ray beam delivery system 55 is fixedly located upstream of the sample holder 16 to allow the first X-ray beam 22 to pass through, and the second X-ray beam delivery system 55 emits a second X-ray beam 58 that is substantially parallel to the first X-ray beam 22. The sample holder 16 can move in a plane perpendicular to the propagation direction Y of the first X-ray beam 22, particularly in a motorized manner, as indicated by the double arrows near the sample holder 16 in Figure 1a and Figure 1b . This allows the sample to be moved from Figure 1a the first X-ray beam 22 in the SAXS configuration shown in Figure 1b to the second X-ray beam 58 in the imaging configuration shown in Figure 1a and Figure 1b . The distal X-ray detector 14 can be used for both configurations, i.e., the configuration for SAXS and the configuration for imaging measurements. Depending on the size of the X-ray detector 14, in addition to the mobility of the X-ray detector 14 along the Y direction, the X-ray detector 14 can be fixed in the XZ plane or can move in the X direction and / or Z direction to intercept the beam 58. In

[0105] In this embodiment of the present invention, the second X-ray beam delivery system 55 is positioned at the entrance of the vacuum chamber 26 that is fixed to a wall directly attached to the vacuum flange (or attached to a reference plate)—i.e., there is no window except for the beryllium exit window of the source 551 at the vertical or horizontal position that is the same as the main collimation path of the first X-ray beam delivery system 12, to isolate the second X-ray source 551. Using a compact X-ray source 551 and a main slit module 56, a distance within the range of 50 mm to 100 mm between the first X-ray beam propagation axis and the second X-ray beam propagation axis can be achieved. Alternatively, if the X-ray source 551 is compact enough, the second X-ray beam delivery system 55 can be placed inside the vacuum chamber 26.

[0106] In Figure 1a and Figure 1b the embodiment shown, the second X-ray beam delivery system 55 has a propagation plane that is parallel to the main propagation plane of the first X-ray beam delivery system 12 and has an inclination included within (-10° < θ < +10°). It can generally be configured to use a sample for measurement at the same position (along the SAXS beam propagation direction Y) as for SAXS measurement, such that the distal X-ray detector 14 can be used to image the sample at the same long distance from the detector for both SAXS and X-ray imaging. In this way, the resolution of X-ray imaging is not or at least less limited by the detector pixel resolution, and the change of the characterization channel becomes simpler and faster. Alternatively, if a trade-off between the search source and the pixel detector resolution is made, X-ray imaging can be performed on samples placed at different positions along the X-ray beam propagation axis Y.

[0107] A small inclination of the propagation plane between the first X-ray beam 22 and the second X-ray beam 58 also ensures that a large field of view (i.e., the measurement sample area) can be achieved while maintaining a large sample-to-detector distance. The distal detector 14 for SAXS is typically a two-dimensional hybrid pixel detector with a pixel size in the range of 55 μm to 172 μm and is mainly designed for SAXS, i.e., it has low noise, a high count rate for measuring absolute intensity, and high efficiency. Generally, the size can be in the range of 30 mm by 75 mm (such as Eiger2R 500K) or 75×75 mm2 (Eiger2R 1M) or up to 150 mm×150 mm (Eiger2R 4M). Regardless of the size of the distal X-ray detector 14 in the prior art SAXS devices, the detector 14 can be motorized in the detector plane, i.e., along the X direction and / or the Z direction, to increase the detection surface at a given sample-to-detector distance or to remove the dead zone within each detector module of the detector assembly. A small inclination of the X-ray imaging beam is required to maintain a large field of view (FOV) of the sample that matches the detector size (FOVdetector = FOVsample * S2 / S1). Alternatively, several exposures are performed for X-ray imaging characterization, where the distal X-ray detector 14 is moved in the XZ plane to increase the detection surface and the field of view of the detector (FOVdetector).

[0108] In an embodiment of the present invention in which the distal X-ray detector 14 is motorized in the XZ plane, the X-ray imaging acquisition may include acquiring a plurality of data exposures by changing the detector position within a range including sub-pixel dimensions. A synthetic image with sub-pixel dimensions can be obtained by convolving the pixel response function and the incident spatial X-ray intensity distribution. For example, by moving the detector half a pixel dimension in both the vertical and horizontal directions, a synthetic image with half the physical pixel dimension can be generated.

[0109] Although the first X-ray beam delivery system 12 typically produces a beam size of usually less than mm2 at the sample, the second X-ray beam delivery system 55 can produce a beam size of up to a few tenths of a millimeter. The inventors have experienced that, although using an X-ray detector 14 with a larger pixel size compared to prior art X-ray imaging systems, X-ray imaging data can be acquired with a resolution of a few micrometers using prior art SAXS systems.

[0110] Positioning the second beam delivery system 55 as shown in the first embodiment of Figure 1a and Figure 1b at the entrance of the vacuum chamber 26 allows for high intensity to be achieved on the sample. However, in the case where the source 55 is too large, different configurations can be selected. This will be described in conjunction with the second embodiment shown in Figure 2 :

[0111] In Figure 2 the second embodiment shown, the X-ray scattering device 10 according to the present invention further includes an insertion module 36 configured to move the second X-ray beam delivery system 55 to a position upstream of the sample holder 16 into the first X-ray beam 22. Further, the main collimator 38 is arranged to extend along the beam path from a position downstream of the first X-ray beam delivery system 12 to a position upstream of the sample holder 16, wherein the insertion module 36 includes a motorized platform 364 configured to alternatively position the second X-ray beam delivery system 55 or the collimator extension 34 into the beam path at a position between the main collimator 38 and the sample holder 16.

[0112] For SAXS measurements, the collimator extension 34 is then positioned in the beam path, allowing the first X-ray beam 22 to be the direct beam incident on the sample mounted on the sample holder 16. However, for imaging measurements, the second X-ray beam delivery system 55 is positioned in the beam path by the motorized platform 364. The computer control system of the X-ray scattering device 10 can then enable the shutter of the first X-ray beam delivery system 12 to block the first X-ray beam 22 while enabling the shutter of the second X-ray beam delivery system 55 to direct the second X-ray beam 58 onto the sample.

[0113] The downstream end of the main collimator 38 and the upstream end of the collimator extension 34 are respectively provided with connection elements for vacuum-tight connection. These connection elements include sliding plates with vacuum-sealing O-rings. This also applies to the downstream end of the collimator extension 34, allowing a vacuum-tight connection to the vacuum chamber 26 at the location where the sample holder 16 is placed. Such a device with connection components 362 and 364 ensures that the interior of the collimator extension 34 is in the same vacuum environment as the interior of the main collimator 38 when the first X-ray beam delivery system 12 or the second X-ray beam delivery system 55 is enabled or during a configuration change, thus ensuring a rapid change of the measurement configuration.

[0114] In an embodiment of the present invention, the connection components 362 and 364 include, for example, sliding plates attached to the collimator extension 34 or attached to the second X-ray beam delivery system 55, which are surrounded by sliding seals to ensure that a vacuum is maintained inside the collimator extension 34 and inside the second beam delivery system 55 at all times, including when the configuration change is completed. The sliding seal is designed to ensure a vacuum-tight connection and low friction when moving along the mating part surface of the sliding plate, which should be flat and smooth. The collimator extension 34 can be a rigid tube or, alternatively, a more flexible system incorporating bellows and more rigid components to facilitate the change of the measurement configuration when the sliding plate moves.

[0115] Alternatively, the collimator extension 34 is provided with a contraction / expansion mechanism. The collimator extension 34 can then be contracted and expanded, for example, by a telescopic mechanism. In the contracted state, the collimator extension 34 can be easily inserted between the main collimator 38 and the sample holder 16 by reducing the friction and contact with the mechanical elements in contact during the movement of the mobile platform 36 holding the collimator extension 34. As long as the collimator extension 34 reaches its final position in the beam path, the collimator extension 34 can be expanded until it contacts the vacuum chamber 26 where the main collimator 38 and / or the sample holder 16 are located or any other optical component arranged upstream of the vacuum chamber 26.

[0116] The propagation directions of the first X-ray beam 22 and the second X-ray beam 58 in the first and second embodiments discussed above are substantially parallel (less than 10°), thus allowing the use of the distal X-ray detector 14 for SAXS and imaging measurements, while Figure 3 A third embodiment of the X-ray scattering device 10 according to the present invention is shown, in which the angle of the propagation direction of the second X-ray beam 58 with respect to the propagation direction Y of the first X-ray beam 22 is greater than 10°. The propagation directions of the two X-ray beams 22, 58 intersect at the sample position.

[0117] In this third embodiment, the second X-ray beam delivery system 55 is located at a position upstream of the sample holder 16 to allow the first X-ray beam 22 to pass through, and further includes a proximal X-ray detector 44 arranged downstream of the sample holder 16 to allow the first X-ray beam 22 to pass through and detect the X-rays transmitted through the sample from the second X-ray beam delivery system 55. As Figure 3 shown, the proximal X-ray detector 44 is located inside the vacuum chamber 26.

[0118] As Figure 3 shown by the dashed arrows in, the sample holder 16 and / or the proximal X-ray detector 44 can rotate, particularly in a motorized manner, about at least one rotation axis passing through the sample holder 16 and perpendicular to the propagation direction of the second X-ray beam 58. In particular, the proximal X-ray detector 44 is preferably capable of moving in a motorized manner along two rotation circles centered on the sample in order to be positioned on a part of the Ewald sphere to collect the scattered signals in the horizontal or vertical directions for X-ray scattering experiments.

[0119] Figure 4 A modification of the second embodiment according to Figure 2 is shown, in which an additional object insertion unit 57 is provided in the vacuum chamber 26 accommodating the sample. The object insertion unit 57 is adapted to mount a random structure object and insert it into the second X-ray beam 58. In Figure 4In the third embodiment shown, the object insertion unit 57 is arranged upstream of the sample holder 16. Alternatively, the object insertion unit 57 may also be arranged downstream of the sample holder 16.

[0120] Positioning the random structure object in the second X-ray beam 58 allows for absorption, phase-contrast, and dark-field imaging measurements to be performed using the distal detector 14 described in detail above, such as speckle-based phase-contrast imaging.

[0121] Of course, the object insertion unit 57 may also be provided in the above-described first and third embodiments.

[0122] For all of the described modes, the X-ray imaging channel may also include the ability to perform a tomography experiment by rotating the sample during X-ray exposure. To this end, the sample holder 16 may include, for example, a vertical rotating stage about the Z-axis for rotating the sample during X-ray exposure with the second X-ray beam 58. In the case of speckle-based phase-contrast imaging, the tomography experiment includes a single exposure in which the random structure object is exposed to the second X-ray beam 58 while the sample is not exposed, and a tomography sequence in which the sample and the random structure object are exposed while the sample is rotated.

[0123] Figure 5 A modification of the second embodiment according to Figure 4 is shown, which is equipped with an additional X-ray beam delivery system that includes an additional X-ray source 30 configured to focus an additional X-ray beam onto a focal spot on or near the sample holder 16 for WAXS measurements. The additional X-ray beam delivery system is also mounted on the motorized platform 36 of the collimator extension 34 and the second X-ray beam delivery system 55. Figure 5 A modification of the X-ray scattering device 10 according to the present invention is shown, which is in a configuration for imaging measurements, in which a conical second X-ray beam 58 irradiates the sample 17 through a random structure object. Of course, the random structure object may also be omitted. Starting from Figure 5 the configuration shown, the movement of the motorized platform 36 in the X direction will first place the X-ray scattering device 10 in its configuration for SAXS measurements, in which the first X-ray beam propagating through the main collimator 38 and the collimator extension 34 will impinge on the sample. Further movement of the motorized platform 36 in the X direction will then place the X-ray scattering device 10 in its configuration for WAXS measurements using the X-ray beam generated by the additional X-ray source 30.

[0124] Such an arrangement allows the use of the first X-ray beam 22 generated by the first X-ray beam delivery system 12 for SAXS measurements, while the use of the further X-ray beam obtained by the further X-ray source 30 for WAXS measurements, including high-resolution WAXS measurements or small sample exposed area scattering applications. Details of such further optimization of the X-ray scattering device 10 for WAXS measurements are described in the applicant's European patent application 19290126.2, the contents of which are incorporated herein by reference.

[0125] In a further development of the invention, the second beam delivery system 55 may comprise a large convergence angle monochromating optic (i.e. 1° for multilayers or several degrees in case of hyperbolic crystals) coupled to a pinhole placed close to the sample position to create a small monochromatic auxiliary source focus. This provides the advantage of modifying the flux / resolution ratio with different pinhole sizes.

[0126] The X-ray generators used in the first X-ray source 18, the second X-ray source 55 and the further X-ray source 30 may comprise a sealed tube X-ray source, preferably a microfocus sealed tube source, or a rotating anode, preferably a point focus, or a liquid jet anode.

[0127] The "focal spot" used throughout the specification and claims need not necessarily be point-shaped. It may also be line-shaped or have a roughly two-dimensional or 3D shape, depending on the respective sample and the intended X-ray scattering analysis.

Claims

1. An X-ray scattering device (10), comprising: - A sample holder (16) for aligning and / or orienting a sample (17) to be analyzed by X-ray scattering; - A first X-ray beam delivery system (12) including a first X-ray source (18) and a first monochromator (20) and arranged upstream of the sample holder (16) for generating and guiding a first X-ray beam (22) along a beam path towards the sample holder (16) in a propagation direction (Y); - A distal X-ray detector (14) arranged downstream of the sample holder (16) and movable along the propagation direction (Y) to detect the first X-ray beam (22) and X-rays scattered from the sample (17) at different scattering angles; - Wherein the first X-ray beam delivery system (12) is configured to focus the first X-ray beam (22) onto a focal spot on or near the distal X-ray detector (14) when placed at a maximum distance from the sample holder (16), or is configured to produce a parallel beam; Characterized in that the X-ray scattering device (10) further comprises a second X-ray beam delivery system (55), the second X-ray beam delivery system (55) including a second X-ray source (551) and configured to generate and guide a divergent second X-ray beam (58) towards the sample holder (16) for X-ray imaging.

2. The X-ray scattering device (10) according to claim 1, characterized in that, The angle of the propagation direction of the second X-ray beam (58) relative to the propagation direction (Y) of the first X-ray beam (22) is less than or equal to 10°.

3. The X-ray scattering device (10) according to claim 1, characterized in that, The second X-ray beam (58) is parallel to the first X-ray beam (22).

4. The X-ray scattering device (10) according to claim 2 or 3, characterized in that, The second X-ray beam delivery system (55) is fixedly located at a position upstream of the sample holder (16) to allow the first X-ray beam (22) to pass through.

5. The X-ray scattering device (10) according to claim 1, characterized in that, The sample holder (16) is movable in a plane perpendicular to the propagation direction (Y) of the first X-ray beam (22).

6. The X-ray scattering device (10) according to claim 2 or 3, characterized in that, The X-ray scattering device (10) further comprises an insertion module (36) configured to move the second X-ray beam delivery system (55) into the first X-ray beam at a position upstream of the sample holder (16).

7. The X-ray scattering device (10) according to claim 6, characterized in that, The X-ray scattering device (10) further comprises a main collimator (38) extending from a position downstream of the first X-ray beam delivery system (12) along the beam path to a position upstream of the sample holder (16), wherein the insertion module (36) includes a motorized platform configured to alternatively position the second X-ray beam delivery system (55) or a collimator extension (34) into the beam path at a position between the main collimator (38) and the sample holder (16).

8. The X-ray scattering device (10) according to claim 7, characterized in that, A corresponding connecting element is provided at the downstream end of the main collimator (38) and the upstream end of the collimator extension (34) for vacuum-tight connection.

9. The X-ray scattering device (10) according to claim 1, wherein, The angle of the propagation direction of the second X-ray beam (58) relative to the propagation direction (Y) of the first X-ray beam (22) is greater than 10°.

10. The X-ray scattering device (10) according to claim 9, characterized in that, The second X-ray beam delivery system (55) is located at a position upstream of the sample holder (16) to allow the first X-ray beam (22) to pass through. In addition, it includes a proximal X-ray detector (44) arranged downstream of the sample holder (16) to allow the first X-ray beam (22) to pass through and detect the X-rays transmitted through the sample (17) from the second X-ray beam delivery system (55).

11. The X-ray scattering device (10) according to claim 10, characterized in that, The sample holder (16) and / or the proximal X-ray detector (44) can rotate about at least one rotation axis passing through the sample holder (16) and perpendicular to the propagation direction of the second X-ray beam (58).

12. The X-ray scattering device (10) according to claim 1, characterized in that, The X-ray scattering device (10) further includes an object insertion unit (57). The object insertion unit (57) is adapted to insert a randomly structured object into the second X-ray beam upstream or downstream of the sample holder (16) to generate an X-ray phase contrast and / or an X-ray dark field image on the distal X-ray detector (14).

13. The X-ray scattering device (10) according to claim 1, characterized in that, The X-ray scattering device (10) further includes an object insertion unit. The object insertion unit is adapted to insert a structured object having a repetitive structure into the second X-ray beam. The structured object is adapted to generate a wavefront modulation of the second X-ray beam, so as to obtain a phase map of the sample by comparing the images generated by the structured object when placed in the beam with and without sample interaction.

14. The X-ray scattering device (10) according to claim 1, characterized in that, The X-ray scattering device (10) further includes a mask insertion unit. The mask insertion unit is adapted to insert a diffraction mask into the second X-ray beam upstream or downstream of the sample holder (16). The diffraction mask is adapted to generate a modulation pattern of the second X-ray beam, so as to generate a two-dimensional dark field image of the sample by comparing the patterns generated by the diffraction mask when placed in the beam with and without sample interaction.

15. The X-ray scattering device (10) according to claim 1, characterized in that, The X-ray scattering device (10) further includes a computer control system configured to control the X-ray scattering device (10) to perform measurements one by one or simultaneously using the first X-ray beam delivery system (12) and the second X-ray beam delivery system (55).

16. An X-ray scattering method using the X-ray scattering device (10) according to any one of the preceding claims, the X-ray scattering method comprising the following steps: - performing X-ray imaging analysis on a sample mounted on the sample holder (16) using the second X-ray beam (58); - defining a region of interest in or on the sample based on the result of the X-ray imaging analysis; and - Perform X-ray scattering analysis on the region of interest using the first X-ray beam (22).

17. The X-ray scattering method according to claim 16, wherein, The X-ray imaging analysis includes combined absorption, phase contrast, and dark field imaging measurements, and wherein the X-ray scattering analysis includes USAXS measurements and / or SAXS measurements and / or WAXS measurements.

Images