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Quasi-two-dimensional (quasi-2D) materials hold promise for future electronics because of their unique band structures that result in electronic and mechanical properties sensitive to crystal strains in all three dimensions. Quantifying crystal strain is a prerequisite to correlating it with the performance of the device and calls for high resolution but spatially resolved rapid characterization methods. Here, we show that using fly-scan nano X-ray diffraction, we can accomplish a tensile strain sensitivity below 0.001% with a spatial resolution of better than 80 nm over a spatial extent of 100 μm on quasi-2D flakes of 1T-TaS2. Coherent diffraction patterns were collected from a ∼100 nm thick sheet of 1T-TaS2 by scanning a 12 keV focused X-ray beam across and rotating the sample. We demonstrate that the strain distribution around micron- and submicron-sized "bubbles" that are present in the sample may be reconstructed from these images. The experiments use state-of-the-art synchrotron instrumentation and will allow rapid and nonintrusive strain mapping of thin-film samples and electronic devices based on quasi-2D materials.

Journal of applied crystallography 53(4), 927 - 936 (2020). doi:10.1107/S1600576720006925, The ever-increasing brightness of synchrotron radiation sources demands improved X-ray optics to utilize their capability for imaging and probing biological cells, nano-devices and functional matter on the nanometre scale with chemical sensitivity. Hard X-rays are ideal for high-resolution imaging and spectroscopic applications owing to their short wavelength, high penetrating power and chemical sensitivity. The penetrating power that makes X-rays useful for imaging also makes focusing them technologically challenging. Recent developments in layer deposition techniques have enabled the fabrication of a series of highly focusing X-ray lenses, known as wedged multi-layer Laue lenses. Improvements to the lens design and fabrication technique demand an accurate, robust, in situ and at-wavelength characterization method. To this end, a modified form of the speckle tracking wavefront metrology method has been developed. The ptychographic X-ray speckle tracking method is capable of operating with highly divergent wavefields. A useful by-product of this method is that it also provides high-resolution and aberration-free projection images of extended specimens. Three separate experiments using this method are reported, where the ray path angles have been resolved to within 4 nrad with an imaging resolution of 45 nm (full period). This method does not require a high degree of coherence, making it suitable for laboratory-based X-ray sources. Likewise, it is robust to errors in the registered sample positions, making it suitable for X-ray free-electron laser facilities, where beam-pointing fluctuations can be problematic for wavefront metrology., Published by Wiley-Blackwell, [S.l.]

Over the last couple of decades, the synchrotron radiation research community has witnessed tremendous advancement in the field of X-ray imaging and microscopy. Continuing enhancement of the light ...

X-ray tomography is widely used for three-dimensional structure determination in many areas of science, from the millimeter to the nanometer scale. The resolution and quality of the 3D reconstruction is limited by the availability of alignment parameters that correct for the mechanical shifts of the sample or sample stage for the images that constitute a scan. In this paper we describe an algorithm for marker-free, fully automated and accurately aligned and reconstructed X-ray tomography data. Our approach solves the tomographic reconstruction jointly with projection data alignment based on a rigid-body deformation model. We demonstrate the robustness of our method on both synthetic phantom and experimental data and show that our method is highly efficient in recovering relatively large alignment errors without prior knowledge of a low resolution approximation of the 3D structure or a reasonable estimate of alignment parameters.

Spectromicroscopy techniques allow the study of local chemical states along with morphology information. At the hard X-ray nanoprobe (HXN) beamline at NSLS-II, we developed nanoscale chemical imaging with high chemical state sensitivity and micron-scale penetration depth. In addition to the chemical images, XRF and phase-contrast images collected simultaneously offer multi-modal, correlative image analysis. We also developed a highly interactive, python-based graphical user interface (NSLS-II MIDAS) that allows multi-modal analysis of nano-XANES and XRF images. Advanced supervised and unsupervised learning algorithms enable users to explore the traditional XANES analysis along with standard machine-learning tools

Diffraction optics fabricated from multilayers offer an intriguing alternative to lithography-based zone plates due to their advantages of virtually limitless aspect ratio and extremely small feature size. However, other issues, intrinsic to thin-film deposition, such as film stress and deposition rate instability , for example, limit the total achievable aperture. Over the last decade, Multilayer Laue Lens (MLLs) have progressed from a mere curiosity with initial aperture sizes in the 3-10 m range, to real beamline-deployed optics with apertures in the 40-50 m range (X. Huang, et al., Scientific Reports 3, 3562 (2013); E. Nazaretski, et al., Rev. Sci. Instrum. 85, 033707 (2014); E. Nazaretski, et al., Journal of Synchrotron Radiation 24, 1113 (2017)). By optimizing deposition conditions and incorporating new materials, MLLs have now broken the 100 m thickness milestone. A flat WSi 2 /Al-Si MLL with a deposition thickness of 102 m, the largest MLL to date, is reviewed. New large aperture wedged MLLs (wMLL), which were first fabricated by APS in 2006 using the WSi 2 /Si material system, are presented which demonstrate high focusing efficiency across a broad energy range. These results confirm findings by other groups who have also independently fabricated wMLL (A. J. Morgan, et al., Scientific Reports 5, 9892 (2015); S. Bajt, et al., Nature Light: Science and Applications 7, 17162 (2017)) based on a similar material system.

Bragg coherent diffractive imaging (BCDI) is a noninvasive microscopy technique that can visualize the morphology and internal lattice deviations of crystals with nanoscale spatial resolution and picometer deformation sensitivity. While BCDI has been successfully applied in various studies of materials, it is less successful for highly strained crystals. Specifically, it is difficult to correctly reconstruct the electron density of a highly strained object using conventional phase retrieval algorithms. Although various algorithms have been developed to overcome this challenge, most of them require a priori knowledge that is not always available in practice. Here we report a phase retrieval workflow that can invert diffraction patterns from multiple Bragg peaks simultaneously. The workflow is explored via simulated diffraction from crystals with various strain conditions. Reconstructions from the workflow consistently demonstrate more accurate electron density maps, in comparison with the conventional method. For highly strained crystals, the workflow improves the reliability and consistency of BCDI phase retrieval significantly.

We report on a developed micromachined silicon platform for the precise assembly of 2D multilayer Laue lenses (MLLs) for high-resolution X-ray microscopy. The platform is 10 &times, 10 mm2 and is fabricated on ~500 &micro, m thick silicon wafers through multiple steps of photolithography and deep reactive-ion etching. The platform accommodates two linear MLLs in a pre-defined configuration with precise angular and lateral position control. In this work, we discuss the design and microfabrication of the platform, and characterization regarding MLLs assembly, position control, repeatability, and stability. The results demonstrate that a micromachined platform can be used for the assembly of a variety of MLLs with different dimensions and optical parameters. The angular misalignment of 2D MLLs is well controlled in the range of the designed accuracy, down to a few millidegrees. The separation distance between MLLs is adjustable from hundreds to more than one thousand micrometers. The use of the developed platform greatly simplifies the alignment procedure of the MLL optics and reduces the complexity of the X-ray microscope. It is a significant step forward for the development of monolithic 2D MLL nanofocusing optics for high-resolution X-ray microscopy.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ∼15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature of a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.

X-ray nanoprobes with 10 nm or sub-10 nm spatial resolution are highly desirable for the next-generation synchrotron beamlines due to the nanoscale imaging capability with high sensitivity to elemental, chemical and structural variations they provide. Multilayer Laue lens (MLL), a type of volume diffractive optics, was shown in theory to be able to focus X-rays to well below 1 nm [1]. In addition to this very high spatial resolution, it can also achieve much higher efficiency than conventional Fresnel zone plate [1]. An MLL is fabricated by sectioning thousands of planar depth-graded layers with nanometer thickness cross-sectionally into several to tens micron thick slivers. The section thickness is critical to achieve the optimum efficiency at desired energy. The requirement of high-aspect-ratio structure of an MLL presents enormous challenges in the post-growth processing, especially as the aperture size (deposition thickness) keeps increasing and therefore the residual stress increases as well. Sectioning without damaging multilayers becomes more and more difficult. At National Synchrotron Light Source II (NSLS-II), we have demonstrated that high quality MLLs can be successfully fabricated by combining mechanical polishing and focused ion beam (FIB) milling. The former removes most of the unwanted material and the latter is used for the fine and final polishing process [2]. MLLs with aperture size of 53 microns made by this method demonstrate around 10 nm focusing capability [3], suggesting that no additional aberration is introduced in the post-growth processing. Wedged MLLs are the best option to achieve sub-10 nm X-ray focusing, because they can produce higher efficiency compared with flat MLLs with the same section thickness [4]. However, sectioning requirement for a wedged MLL is more stringent because best focusing of a wedged MLL (in terms of both focus size and efficiency) can only achieved at a specific section thickness for one optimized energy. In this presentation, I will introduce the process, advantages, and technical difficulties of using the combined mechanical polishing and FIB method to make MLLs. The strategies to tackle the problems and make site-specific wedged MLLs will also be presented. [1] J. Maser, G.B. Stephenson, S. Vogt, W. Yun, A. T. Macrander, H. C. Kang, C. Liu, and R. Conley, “Multilayer Laue lenses as high-resolution x-ray optics”, in Design and Microfabrication of Novel X-Ray Optics II, edited by A. Snigirev, D. Mancini, Proc. SPIE 5539, 185-194, SPIE, Bellingham, WA, (2004) [2] H. Yan, R. Conley, N. Bouet, and Y. S. Chu, “Hard x-ray nanofocusing by multilayer Laue lenses”, Journal of Physics D: Applied Physics 47, 263001 (2014) [3] H. Yan, N. Bouet, J. Zhou, X. J. Huang, E. Nazaretski, W. H. Xu, A. P. Cocco, W. K. S. Chiu, K. S. Brinkman and Y. S. Chu, “Multimodal hard x-ray imaging with resolution approaching 10nm for studies in material science”, Nano Futures, 2, 011001 (2018) [4] H. Yan, J. Maser, A. Macrander, Q. Shen, S. Vogt, G. Stephenson, and H. Kang, “Takagi-Taupin description of x-ray dynamical diffraction from diffractive optics with large numerical aperture”, Phys. Rev. B, 76, 115438 (2007).

Scanning hard x-ray microscopy is a versatile imaging tool that offers a suite of analytic x-ray techniques for studying spatially-resolved elemental, structural and chemical variations. Recent advances in nano-focusing optics and instrumentation have pushed the frontier of the field into multi-modal imaging in 3D and with nanoscale resolution. Here we present current imaging capabilities provided by the hard x-ray nanoprobe of the National Synchrotron Light Source II at Brookhaven National Laboratory. A variety of imaging modalities (absorption, phase, fluorescence and diffraction) will be discussed, as well as the data analysis challenges associated with them. We show that x-ray imaging at about 10 nm resolution has become routine measurements at the beamline, and has been used for a wide spectrum of scientific applications.

X-ray microscopy is a mature characterization tool routinely used to answer various questions of science, technology and engineering. The high penetration power of X-rays allows to utilize different characterization methods and reveal elemental composition, crystalline phases, strain distribution, oxidation states etc. in macroscopic and microscopic samples. To obtain comprehensive chemical and structural information at the nanometer scale an X-ray microscope must be equipped with adequate capabilities and allow acquisition of multiple datasets simultaneously. Full-field or scanning X-ray microscopes usually serve this purpose and complement each other. In the recent years, a number of X-ray microscopes have been designed, constructed and commissioned at NSLS-II. In this work we provide an overview of the microscopy instrumentation developments at NSLS-II. It includes the multilayer Laue Lens based nanoprobe optimized for 10 nm spatial resolution imaging, it’s current status and future upgrades; the zone plate based full-field imaging system capable of nano-tomography measurements in less than 1 minute; a laser scanning system optimized for ptychography measurements along with algorithms development, and a new Kirkpatrick-Baez based scanning microscope designed for sub-100 nm spatial resolution experiments.

Hard X-ray microscopy is a powerful scientific tool capable of providing sub-10 nm spatial resolution imaging of material’s chemical composition and internal structure. Multilayer Laue Lenses (MLLs) have been developed and used for hard x-ray nanofocusing. MLLs are one dimensional X-ray diffractive optics fabricated through multilayer deposition and sectioning. An orthogonal alignment of two MLLs yields a point focus; 10 milli-degree orthogonality and sub-10 µm positioning accuracy along the beam direction is required to avoid astigmatism and achieve 10 nm focal spot size at 12 keV photon energy. Up-to-date, developed x-ray microscopy systems were equipped with eight degrees of nano-scale motion to perform full alignment of individual MLL optics. Bonding of two individual lenses together in pre-determined configuration significantly simplifies alignment process and makes them compatible with a more conventional Zone Plate – based microscopes. In this work, we give an overview of the existing bonding effort and present our approach to fabricate a monolithic 2D MLL optic.

We report on the development of 2D integrated multilayer Laue lens (MLL) nanofocusing optics used for high-resolution x-ray microscopy. A Micro-Electro-Mechanical-Systems (MEMS) - based template has been designed and fabricated to accommodate two linear MLL optics in pre-aligned configuration. The orthogonality requirement between two MLLs has been satisfied to a better than 6 millidegrees level, and the separation along the x-ray beam direction was controlled on a micrometer scale. Developed planar 2D MLL structure has demonstrated astigmatism free point focus of ∼14 nm by ∼13 nm in horizontal and vertical directions, respectively, at 13.6 keV photon energy. Approaching 10 nm resolution with integrated 2D MLL optic is a significant step forward in applications of multilayer Laue lenses for high-resolution hard x-ray microscopy and their adoption by the general x-ray microscopy community.

International audience; III-As nanowires are candidates for near infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nano-focused x-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largely unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multi-angle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of x-ray radiation, together with the relaxed constraints of maBPP, will enable in operado imaging of nanowire devices.

Hard X-ray microscopy is a prominent tool suitable for nanoscale-resolution non-destructive imaging of various materials used in different areas of science and technology. With an ongoing effort to push the 2D/3D imaging resolution down to 10 nm in the hard X-ray regime, both the fabrication of nano-focusing optics and the stability of the microscope using those optics become extremely challenging. In this work a microscopy system designed and constructed to accommodate multilayer Laue lenses as nanofocusing optics is presented. The developed apparatus has been thoroughly characterized in terms of resolution and stability followed by imaging experiments at a synchrotron facility. Drift rates of ∼2 nm h−1accompanied by 13 nm × 33 nm imaging resolution at 11.8 keV are reported.

We discuss misalignment-induced aberrations in a pair of crossed multilayer Laue lenses used for achieving a nanometer-scale x-ray point focus. We thoroughly investigate the impacts of two most important contributions, the orthogonality and the separation distance between two lenses. We find that misalignment in the orthogonality results in astigmatism at 45° and other inclination angles when coupled with a separation distance error. Theoretical explanation and experimental verification are provided. We show that to achieve a diffraction-limited point focus, accurate alignment of the azimuthal angle is required to ensure orthogonality between two lenses, and the required accuracy is scaled with the ratio of the focus size to the aperture size.

We report scanning hard x-ray imaging with a monolithic focusing optic consisting of two multilayer Laue lenses (MLLs) bonded together. With optics pre-characterization and accurate control of the bonding process, we show that a common focal plane for both MLLs can be realized at 9.317 keV. Using bonded MLLs, we obtained a scanning transmission image of a star test pattern with a resolution of 50 × 50 nm2. By applying a ptychography algorithm, we obtained a probe size of 17 × 38 nm2 and an object image with a resolution of 13 × 13 nm2. The significant reduction in alignment complexity for bonded MLLs will greatly extend the application range in both scanning and full-field x-ray microscopies.

The article presents a theoretical study on dynamic artefacts in the reconstruction of Bragg coherent diffractive imaging using an iterative phase retrieval algorithm., This article reports a theoretical study on the reconstruction artefacts in Bragg coherent diffractive imaging caused by dynamical diffraction effects. It is shown that, unlike the absorption and refraction effects that can be corrected after reconstruction, dynamical diffraction effects have profound impacts on both the amplitude and the phase of the reconstructed complex object, causing strong artefacts. At the dynamical diffraction limit, the reconstructed shape is no longer correct, as a result of the strong extinction effect. Simulations for hemispherical particles of different sizes show the type, magnitude and extent of the dynamical diffraction artefacts, as well as the conditions under which they are negligible.

In this study, the sampling statistics of X-ray diffraction data obtained from polycrystalline nanopowders are studied through analytical formulations and numerical modelling. It is shown that the very large acceptance angles of crystalline nanoparticles can cause issues in computing the number of diffracting grains scattering into a given Bragg reflection. These results intimate that formulations previously tested and verified for polycrystalline aggregates with grains larger than 500 nm should be revalidated for particles with coherent scattering lengths below 10 nm.

This publisher's note corrects an error in Eq. (3) of Opt. Lett.44, 503 (2019).OPLEDP0146-959210.1364/OL.44.000503.

Ptychography is a scanning variation of the coherent diffractive imaging method for providing high-resolution quantitative images from specimen with extended dimensions. Its capability of achieving diffraction-limited spatial resolution can be compromised by the sample thickness, which is generally required to be thinner than the depth of field of the imaging system. In this Letter, we present a method to extend the depth of field for ptychography by numerically generating the focus stack from reconstructions with propagated illumination wavefronts and combining the in-focus features to a single sharp image using an algorithm based on the complex-valued discrete wavelet transform. This approach does not require repeated measurements by translating the sample along the optical axis as in the conventional focus stacking method, and offers a computation-efficient alternative to obtain high-resolution images with extended depth of fields, complementary to the multi-slice ptychography.

The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever increasing source brightness, which have significantly advanced ex-situ and in-situ research for energy materials, such as lithium-ion batteries. However, the strong beam-matter interaction arisen from the high beam flux can significantly modify the material structure. The parasitic beam-induced effect inevitably interferes with the intrinsic material property, which brings difficulties in interpreting experimental results, and therefore requires comprehensive evaluation. Here we present a quantitative in-situ study of the beam-effect on one electrode material Ag2VO2PO4 using four different X-ray probes with different radiation dose rate. The material system we reported exhibits interesting and reversible radiation-induced thermal and chemical reactions, which was further evaluated under electron microscopy to illustrate the underlying mechanism. The work we presented here will provide a guideline in using synchrotron X-rays to distinguish the materials’ intrinsic behavior from extrinsic structure changed induced by X-rays, especially in the case of in-situ and operando study where the materials are under external field of either temperature or electric field.

We developed a scanning hard x-ray microscope using a new class of x-ray nano-focusing optic called a multilayer Laue lens and imaged a chromosome with nanoscale spatial resolution. The combination of the hard x-ray’s superior penetration power, high sensitivity to elemental composition, high spatial-resolution and quantitative analysis creates a unique tool with capabilities that other microscopy techniques cannot provide. Using this microscope, we simultaneously obtained absorption-, phase- and fluorescence-contrast images of Pt-stained human chromosome samples. The high spatial-resolution of the microscope and its multi-modality imaging capabilities enabled us to observe the internal ultra-structures of a thick chromosome without sectioning it.

Commissioning of the first X-ray beamlines of NSLS-II included detailed measurements of spectral and spatial distributions of the radiation at different locations of the beamlines, from front-ends to sample positions. Comparison of some of these measurement results with high-accuracy calculations of synchrotron (undulator) emission and wavefront propagation through X-ray transport optics, performed using SRW code, is presented.

We report on an ongoing project to create a portable tomography toolbox to enable the processing of user data on various computing platforms. Our goal is to create a collection of open source software applications in a single integrated package that is cross-platform, to facilitate analysis and interpretation of tomographic data emerging from the Brookhaven National Synchrotron Light Source (NSLS) II and Center for Functional Nanomaterials (CFN) facilities as well as other locations. The emerging container technology Docker makes it possible to integrate independent software packages in a single toolbox and allows us to abstract away the library and platform dependencies from the user’s point of view and develop a portable toolbox. To demonstrate, we Dockerized TomoPy and tomo display, two popular tomographic image processing software packages, and used them to analyze the images obtained at the NSLS X2B beam line. We also report some advances in the artifact-removal algorithms which will be an integral part of the preprocessing stage for the tomography toolbox.

The Hard X-ray Nanoprobe (HXN) beamline at NSLS-II has been designed and constructed to enable imaging experiments with unprecedented spatial resolution and detection sensitivity. The HXN X-ray Microscope is a key instrument for the beamline, providing a suite of experimental capabilities which includes scanning fluorescence, diffraction, differential phase contrast and ptychography utilizing Multilayer Laue Lenses (MLL) and zoneplate (ZP) as nanofocusing optics. We present technical requirements for the MLL-based scanning microscope, outline the development concept and present first ∼15 × 15 nm2 spatial resolution x-ray fluorescence images.

Multilayer Laue lenses (MLLs) have demonstrated great capabilities for efficiently focusing hard X-rays down to the nanometer scale. Optimized use of MLLs in a scanning X-ray microscope requires careful consideration of a number of practical parameters other than resolution and efficiency in order to optimize the microscope's performance and scientific throughput. Here, relationships among the apodization effect owing to the presence of a beamstop, the monochromaticity requirement and the allowable working distance are discussed, as well as their impacts on the performance of the optics. Based on these discussions, optimal MLL schemes aiming at 10 nm resolution for a scanning X-ray microscope for the Hard X-ray Nanoprobe (HXN) beamline at National Synchrotron Light Source II are presented.

Ultra-low emittance third-generation synchrotron radiation (SR) sources, such as NSLS-II and MAX-IV, will offer excellent opportunities for further development of experimental techniques exploiting X-ray coherence. However, even in these new SR sources, the radiation produced by relativistic electrons (in undulators, wigglers and bending magnets) will remain only partially coherent in the X-ray spectral range. “Extraction” of “coherent portion” of the radiation flux and its transport to sample without loss of coherence must be performed by dedicated SR beamlines, optimized for particular types of experiments. Detailed quantitative prediction of partially coherent X-ray beam properties at propagation through optical elements, which is required for the optimization of such beamlines, can only be obtained from accurate and efficient physical-optics based numerical simulations. Examples of such simulations, made for NSLS-II beamlines, using “Synchrotron Radiation Workshop” (SRW) computer code, are presented. Special attention is paid to the numerical analysis of the basic properties of partially coherent undulator radiation beam and its distinctions from the Gaussian beam. Performance characteristics of importance for particular beamlines, such as radiation spot size and flux at sample vs size of secondary source aperture for high-resolution microscopy beamlines, are predicted by the simulations.

The multilayer Laue lens (MLL) is a novel diffractive optic for hard X-ray nanofocusing, which is fabricated by thin film deposition techniques and takes advantage of the dynamical diffraction effect to achieve a high numerical aperture and efficiency. It overcomes two difficulties encountered in diffractive optics fabrication for focusing hard X-rays: (1) small outmost zone width and (2) high aspect ratio. Here, we will give a review on types, modeling approaches, properties, fabrication, and characterization methods of MLL optics. We show that a full-wave dynamical diffraction theory has been developed to describe the dynamical diffraction property of the MLL and has been employed to design the optimal shapes for nanofocusing. We also show a 16 nm line focus obtained by a partial MLL and several characterization methods. Experimental results show a good agreement with the theoretical calculations. With the continuing development of MLL optics, we believe that an MLL-based hard x-ray microscope with true nanometer resolution is on the horizon.

We report multimodal scanning hard x-ray imaging with spatial resolution approaching 10 nm and its application to contemporary studies in the field of material science. The high spatial resolution is achieved by focusing hard x-rays with two crossed multilayer Laue lenses and raster-scanning a sample with respect to the nanofocusing optics. Various techniques are used to characterize and verify the achieved focus size and imaging resolution. The multimodal imaging is realized by utilizing simultaneously absorption-, phase-, and fluorescence-contrast mechanisms. The combination of high spatial resolution and multimodal imaging enables a comprehensive study of a sample on a very fine length scale. In this work, the unique multimodal imaging capability was used to investigate a mixed ionic-electronic conducting ceramic-based membrane material employed in solid oxide fuel cells and membrane separations (compound of Ce0.8Gd0.2O2−x and CoFe2O4) which revealed the existence of an emergent material phase and quantified the chemical complexity at the nanoscale.

The presence of strain distributions within semiconductor features influences many aspects of their behavior. For example, microelectronic technology that incorporates strained silicon improves device performance by increasing carrier mobility in the Si channels. Because current semiconductor fabrication contains multiple levels of metallic and dielectric structures, an understanding of the mechanical response of the constituent elements is critical to the prediction of the overall device performance. In addition, the interaction of strain fields between adjacent structures becomes greater as feature sizes decrease and the corresponding feature density increases. The use of synchrotron-based X-ray methods allows one to determine the interaction between strained features and their environment at a submicron resolution. Real-space mapping of strain distributions in pseudomorphically strained, raised SiGe structures revealed that elastic relaxation extends approximately 20 times the feature thickness from their edges. X-ray topographic methods were also applied to map the substrate deformation induced by overlying SiGe features. A formulation based on the classical Ewald-von Laue theory of dynamical diffraction was derived to match the measured diffraction profiles.

This work presents a set of equations that can be used to predict the dynamical diffraction profile from a non-transparent single crystal with a constant strain gradient examined in Bragg reflection geometry with a spherical incident X-ray beam. In agreement with previous work, the present analysis predicts two peaks: a primary diffraction peak, which would have still been observed in the absence of the strain gradient and which exits the specimen surface at the intersection point of the incident beam with the sample surface, and a secondary (mirage) peak, caused by the deflection of the wavefield within the material, which exits the specimen surface further from this intersection point. The integrated intensity of the mirage peak increases with increasing strain gradient, while its separation from the primary reflection peak decreases. The directions of the rays forming the mirage peak are parallel to those forming the primary diffraction peak. However, their spatial displacement might cause (fictitious) angular shifts in diffractometers equipped with area detectors or slit optics. The analysis results are compared with experimental data from an Si single-crystal strip bent in cantilever configuration, and the implications of the mirage peak for Laue analysis and high-precision diffraction measurements are discussed.

We report on the fabrication and the characterization of a wedged multilayer Laue lens for x-ray nanofocusing. The lens was fabricated using a sputtering deposition technique, in which a specially designed mask was employed to introduce a thickness gradient in the lateral direction of the multilayer. X-ray characterization shows an efficiency of 27% and a focus size of 26 nm at 14.6 keV, in a good agreement with theoretical calculations. These results indicate that the desired wedging is achieved in the fabricated structure. We anticipate that continuous development on wedged MLLs will advance x-ray nanofocusing optics to new frontiers and enrich capabilities and opportunities for hard X-ray microscopy.

Diffraction profiles from an Si-single-crystal strip deformed in cantilever bending are presented as a function of tip displacement and incident-beam energy. Data obtained with slit-based diffracted-beam optics contain a secondary peak in addition to the primary 004 reflection for all energies when the bending strain is finite. This secondary peak can be identified as a `mirage' peak, predicted by dynamical diffraction theory to occur in weakly deformed single-crystal samples. The integrated intensity of this mirage peak increases with increasing energy and tip displacement and exceeds the primary peak intensity at higher values. The mirage peak disappears when a monochromator is used in the diffracted-beam path. Data that show the effect of these mirage peaks on X-ray diffraction strain analysis are presented, and it is shown that a diffracted-beam monochromator may be used to eliminate these errors.

Non-invasive techniques such as electrical capacitance tomography (ECT) are beginning to make promising contributions to control systems and are well fitted for flow-regime identification in opaque pipes or conduits. A new method of two-component flow-regime identification based on a neural network and an eight-electrode ECT sensor is proposed in this paper. Time-consuming image reconstruction and analysis are avoided. Ten feature parameters are extracted straight from the capacitance measurements and translated into regime information via a back-propagation (BP) network. The extraction of feature parameters, the architecture and the training of the BP network are given. Simulation results show that the new identification method has good precision and high speed. The use of feature parameters and the BP network for flow-regime identification is promising.

Multilayer Laue lenses (MLLs) are x-ray focusing optics with the potential to focus hard x-rays down to a single nanometer level. In order to achieve point focus, an MLL microscope needs to have the capability to perform tip-tilt motion of MLL optics and to hold the angular position for an extended period of time. In this work, we present a 2D tip-tilt system that can achieve an angular resolution of over 100 microdegree with a working range of 4°, by utilizing a combination of laser interferometer and mini retroreflector. The linear dimensions of the developed system are about 30 mm in all directions, and the thermal dissipation of the system during operation is negligible. Compact design and high angular resolution make the developed system suitable for MLL optics alignment in the next generation of MLL-based x-ray microscopes.

We report on the synthesis, stability, and local structure of In2O3 thin films grown via rf-magnetron sputtering and characterized by in-situ x-ray scattering and focused x-ray nanodiffraction. We find that In2O3 deposited onto (0 0 1)-oriented single crystal yttria-stabilized zirconia substrates adopts a Stranski–Krastanov growth mode at a temperature of 850 °C, resulting in epitaxial, truncated square pyramids with (1 1 1) side walls. We find that at this temperature, the pyramids evaporate unless they are stabilized by a low flux of In2O3 from the magnetron source. We also find that the internal lattice structure of one such pyramid is made up of differently strained volumes, revealing local structural heterogeneity that may impact the properties of In2O3 nanostructures and films.

In this study,we present a numerical framework for modeling three-dimensional (3D) diffraction data in Bragg coherent diffraction imaging (BraggCDI) experiments and evaluating the quality of obtained 3D complex-valued real-space images recovered by reconstruction algorithms under controlled conditions. The approach is used to systematically explore the performance and the detection limit of this phase-retrieval-based microscopy tool. The numerical investigation suggests that the superb performance of Bragg CDI is achieved with an oversampling ratio above 30 and a detection dynamic range above 6 orders. The observed performance degradation subject to the data binning processes is also studied. This numerical tool can be used to optimize experimental parameters and has the potential to significantly improve the throughput of Bragg CDI method.

We report our experiences with conducting ptychography simultaneously with the X-ray fluorescence measurement using the on-the-fly mode for efficient multi-modality imaging. We demonstrate that the periodic artifact inherent to the raster scan pattern can be mitigated using a sufficiently fine scan step size to provide an overlap ratio of >70%. This allows us to obtain transmitted phase contrast images with enhanced spatial resolution from ptychography while maintaining the fluorescence imaging with continuous-motion scans on pixelated grids. This capability will greatly improve the competence and throughput of scanning probe X-ray microscopy.

We have designed and constructed a dedicated instrument to perform ptychography measurements and characterization of multilayer Laue lenses nanofocusing optics. The design of the scanning microscope provides stability of components and minimal thermal drifts, requirements for nanometer scale spatial resolution measurements. We performed thorough laboratory characterization of the instrument in terms of resolution and thermal drifts with subsequent measurements at a synchrotron. We have successfully acquired and reconstructed ptychography data yielding 11 nm line focus.

We have fabricated partial Multilayer Laue Lens (MLL) linear zone plate structures with thousands of alternating WSi2 and Si layers and various outermost zone widths according to the Fresnel zone plate formula. Using partial MLL structures, we were able to focus hard X-rays to line foci with a width of 30 nm and below. Here, we describe challenges and approaches used to bond these multilayers to achieve line and point focusing. Bonding was done by coating two multilayers with AuSn and heating in a vacuum oven at 280–3001C. X-ray reflectivity measurements confirmed that there was no change in the multilayers after heating to 3501C. A bonded MLL was polished to a 5–25mm wedge without cracking. SEM image analyses found well-positioned multilayers after bonding. These results demonstrate the feasibility of a bonded full MLL for focusing hard X-rays. r 2007 Published by Elsevier B.V.

We present a simulation result of the focusing performance of a multilayer Laue lens (MLL) with imperfections. Imperfections we have studied correspond to deviations of sequence of layers in the fabricated structure from the zone plate law. The actual sequence of layers of the MLL is measured by scanning electron microscope (SEM), and fitted by second order polynomials. X-ray characterization of the MLL structures is performed using coherent X-rays at the Advanced Photon Source. We observe very good agreement between experiment and simulation. This demonstrates that our simulation method can serve as an efficient tool to characterize the focusing performance of MLLs with imperfections, and thereby allows us to provide feedback following deposition and fabrication of the MLL structures and optimization of focusing structures prior to X-ray characterization.

The focusing performance of a multilayer Laue lens (MLL) with 43.4 μm aperture, 4 nm finest zone width and 4.2 mm focal length at 12 keV was characterized with X-rays using ptychography method. The reconstructed probe shows a full-width-at-half-maximum (FWHM) peak size of 11.2 nm. The obtained X-ray wavefront shows excellent agreement with the dynamical calculations, exhibiting aberrations less than 0.3 wave period, which ensures the MLL capable of producing a diffraction-limited focus while offering a sufficient working distance. This achievement opens up opportunities of incorporating a variety of in-situ experiments into ultra high-resolution X-ray microscopy studies.

Fresnel Zone Plates (FZP) are to date very successful focusing optics for X-rays. Established methods of fabrication are rather complex and based on electron beam lithography (EBL). Here, we show that ion beam lithography (IBL) may advantageously simplify their preparation. A FZP operable from the extreme UV to the limit of the hard X-ray was prepared and tested from 450 eV to 1500 eV. The trapezoidal profile of the FZP favorably activates its 2nd order focus. The FZP with an outermost zone width of 100 nm allows the visualization of features down to 61, 31 and 21 nm in the 1st, 2nd and 3rd order focus respectively. Measured efficiencies in the 1st and 2nd order of diffraction reach the theoretical predictions.