X-ray Interferometer Research Articles

Multi-image X-ray interferometer module: II. Demonstration of high-resolution X-ray imaging with regular-interval coded apertures

Multi-image X-ray interferometer module: II. Demonstration of high-resolution X-ray imaging with regular-interval coded apertures

Monolithic deformable mirror based on lithium niobate single crystal for high-resolution X-ray adaptive microscopy

X-ray microscopy is very promising not only for nondestructive and high-spatial-resolution observation of the internal structure of a sample but also for elemental distribution and chemical state analysis. However, the spatial resolution of microscopes remains unsatisfactory owing to the fabrication error in the objective lens. To realize an ultra-high-resolution, we propose and develop a monolithic deformable mirror based on a lithium niobite single crystal and a novel adaptive imaging system based on it. An X-ray interferometer confirmed that shape modification is possible with an accuracy of 0.67 nm in peak to valley under high stability (0.17 nm over 7 h) and hysteresis-free deformation control. Introducing this adaptive mirror into an X-ray microscope based on advanced Kirkpatrick-Baez mirror optics and correcting the wavefront aberration demonstrated that the X-ray image quality could be significantly improved.

A four-grating interferometer for x-ray multi-contrast imaging.

X-ray multi-contrast imaging with gratings provides a practical method to detect differential phase and dark-field contrast images in addition to the x-ray absorption image traditionally obtained in laboratory or hospital environments. Systems have been developed for preclinical applications in areas including breast imaging, lung imaging, rheumatoid arthritis hand imaging and kidney stone imaging. Prevailing x-ray interferometers for multi-contrast imaging include Talbot-Lau interferometers and universal moiré effect-based phase-grating interferometers. Talbot-Lau interferometers suffer from conflict between high interferometer sensitivity and large field of view (FOV) of the object being imaged. A small period analyzer grating is necessary to simultaneously achieve high sensitivity and large FOV within a compact imaging system but is technically challenging to produce for high x-ray energies. Phase-grating interferometers suffer from an intrinsic fringe period ranging from a few micrometers to several hundred micrometers that can hardly be resolved by large area flat panel x-ray detectors. The purpose of this work is to introduce a four-grating x-ray interferometer that simultaneously allows high sensitivity and large FOV, without the need for a small period analyzer grating. The four-grating interferometer consists of a source grating placed downstream of and close to the x-ray source, a pair of phase gratings separated by a fixed distance placed downstream of the source grating, and an analyzer grating placed upstream of and close to the x-ray detector. The object to be imaged is placed upstream of and close to the phase-grating pair. The distance between the source grating and the phase-grating pair is designed to be far larger than that between the phase-grating pair and the analyzer grating to promote simultaneously high sensitivity and large FOV. The method was evaluated by constructing a four-grating interferometer with an 8µm period source grating, a pair of phase gratings of 2.4µm period, and an 8µm period analyzer grating. The fringe visibility of the four-grating interferometer was measured to be ≈24% at 40kV and ≈18% at 50kV x-ray tube operating voltage. A quartz bead of 6mm diameter was imaged to compare the theoretical and experimental phase contrast signal with good agreement. Kidney stone specimens were imaged to demonstrate the potential of such a system for classification of kidney stones. The proposed four-grating interferometer geometry enables a compact x-ray multi-contrast imaging system with simultaneously high sensitivity and large FOV. Relaxation of the requirement for a small period analyzer grating makes it particularly suitable for high x-ray energy applications such as abdomen and chest imaging.

Measurements of the geometrical characteristics and refractive index of specimens made with X-ray interferometers

The theoretical background to the formation of interference fringes in a triple Laue X-ray interferometer by a specimen having plano-concave form is presented. The interference fringes in the general case have an elliptical form. The relation between the radius of the specimen, the refractive index and the radii of the interference fringes is established. For two epoxy lenses having different radii, the interference fringes are registered. The refractive index and the radii are determined by measuring the radii of the obtained interference fringes.

Optical development in the murine eye lens of accelerated senescence-prone SAMP8 and senescence-resistant SAMR1 strains

The eye lens is responsible for focusing objects at various distances onto the retina and its refractive power is determined by its surface curvature as well as its internal gradient refractive index (GRIN). The lens continues to grow with age resulting in changes to the shape and to the GRIN profile. The present study aims to investigate how the ageing process may influence lens optical development. Murine lenses of accelerated senescence-prone strain (SAMP8) aged from 4 to 50 weeks; senescence-resistant strain (SAMR1) aged from 5 to 52 weeks as well as AKR strain (served as control) aged from 6 to 70 weeks were measured using the X-ray interferometer at the SPring-8 synchrotron Japan within three consecutive years from 2020 to 2022. Three dimensional distributions of the lens GRIN were reconstructed using the measured data and the lens shapes were determined using image segmentation in MatLab. Variations in the parameters describing the lens shape and the GRIN profile with age were compared amongst three mouse strains. With advancing age, both the lens anterior and posterior surface flattens and the lens sagittal thickness increase in all three mouse strains (Anterior radius of curvature increase at 0.008 mm/week, 0.007 mm/week and 0.002 mm/week while posterior radius of curvature increase at 0.002 mm/week, 0.007 mm/week and 0.003 mm/week respectively in AKR, SAMP8 and SAMR1 lenses). Compared with the AKR strain, the SAMP8 samples demonstrate a higher rate of increase in the posterior curvature radius (0.007 mm/week) and the thickness (0.015 mm/week), whilst the SAMR1 samples show slower increases in the anterior curvature radius (0.002 mm/week) and its thickness (0.013 mm/week). There are similar age-related trends in GRIN shape in the radial direction (in all three types of murine lenses nr2 and nr6 increase with age while nr4 decrease with age consistently) but not in the axial direction amongst three mouse strains (nz1 of AKR lens decrease while of SAMP8 and SAMR1 increase with age; nz2 of all three models increase with age; nz3 of AKR lens increase while of SAMP8 and SAMR1 decrease with age). The ageing process can influence the speed of lens shape change and affect the GRIN profile mainly in the axial direction, contributing to an accelerated decline rate of the optical power in the senescence-prone strain (3.5 D/week compared to 2.3 D/week in the AKR control model) but a retardatory decrease in the senescence-resistant strain (2.1 D/week compared to the 2.3D/week in the AKR control model).

Investigation of the Effect of Defocusing on the Interference Patterns Obtained Using Three-Block X-ray Interferometers

Investigation of the Effect of Defocusing on the Interference Patterns Obtained Using Three-Block X-ray Interferometers

Multi-image x-ray interferometer module: I. Design concept and proof-of-concept experiments with fine-pitch slits

We propose an x-ray imaging system, multi-image x-ray interferometer module (MIXIM), with which a very high angular resolution can be achieved even with a small system size. MIXIM is composed of equally spaced multiple slits and an x-ray detector, and its angular resolution is inversely proportional to the distance between them. Here, we report our evaluation experiments of MIXIM with a newly adopted CMOS sensor with a high spatial resolution of 2.5 μm. Our previous experiments with a prototype MIXIM were limited to one-dimensional imaging, and more importantly, the achieved angular resolution was only ∼1 ″ , severely constrained due to the spatial resolution of the adopted sensor with a pixel size of 4.25 μm. By contrast, one-dimensional images obtained in this experiment had a higher angular resolution of 0.5″ when a configured system size was only ∼1 m, which demonstrates that MIXIM can simultaneously realize a high angular resolution and compact size. We also successfully obtained a two-dimensional profile of an x-ray beam for the first time for MIXIM by introducing a periodic pinhole mask. The highest angular resolution achieved in our experiments is smaller than 0.1″ with a mask-sensor distance of 866.5 cm, which shows the high scalability of MIXIM.

Crystal bending in triple-Laue X-ray interferometry. Part II. Phase-contrast topography.

In a previous paper [Sasso et al. (2023). J. Appl. Cryst.56, 707-715], the operation of a triple-Laue X-ray interferometer having the splitting or recombining crystal cylindrically bent was studied. It was predicted that the phase-contrast topography of the interferometer detects the displacement field of the inner crystal surfaces. Therefore, opposite bendings result in the observation of opposite (compressive or tensile) strains. This paper reports on the experimental confirmation of this prediction, where opposite bendings were obtained by copper deposition on one or the other of the crystal sides.

Crystal-Based X-ray Interferometry and Its Application to Phase-Contrast X-ray Imaging, Zeff Imaging, and X-ray Thermography

Crystal-based X-ray interferometry (CXI) detects X-ray phase shifts by using the superposition of waves, and its sensitivity is the highest among the other X-ray phase-detecting methods. Therefore, phase-contrast X-ray imaging (PCXI) using CXI has the highest density resolution among the PCXI methods and enables fine, non-destructive observation with a density resolution below sub-mg/cm3. It has thus been applied in a wide range of fields, including biology, medicine, geology, and industry, such as visualization of the testis and brains of aged rats with tumors, human embryos at each Carnegie stage, air hydrates in old Antarctic ice, and ion distribution in electrolytes. Novel imaging methods have also been developed to take advantage of its high sensitivity, such as visualization of the effective atomic number (Zeff) and the three-dimensional temperature of samples. This article reviews the principles and history of PCXI and crystal-based X-ray interferometers, as well as a CXI system using synchrotron radiation and its potential applications from biomedical to industrial.

Fringe visibility in X-ray interferometer using dual triangular phase gratings

In recent years, the X-ray interferometer using dual phase gratings has been extensively studied. The large periodic fringes produced by the X-ray interferometer using dual phase gratings can be directly detected by ordinary detectors. At the same time, the X-ray interferometer using dual phase gratings can reduce the radiation dose of the sample without using absorption gratings. Meanwhile, a high fringe visibility is always preferred to achieve a high signal-to-noise ratio for X-ray grating interferometry. However, recent studies have reported that experimental fringe visibility in X-ray interferometer using dual rectangular phase gratings is relatively low. Therefore, it is necessary to further increase the fringe visibility in X-ray interferometry using dual phase gratings. This work focuses on the analysis of fringe visibility in X-ray interferometer using dual triangular phase gratings. Based on the fringe intensity distribution formula of X-ray dual phase grating interferometer, the fringe visibility of the dual triangular phase grating interferometer is investigated as a function of the grating spacing under monochromatic and polychromatic illumination, respectively. For comparison, the fringe visibility of the dual rectangular phase grating interferometer is also studied under the same condition. The results show that the maximum fringe visibility of the dual triangular phase grating interferometer increases with the phase shift increasing regardless of monochromatic or polychromatic illumination. Under monochromatic illumination, the maximum fringe visibility of dual 5π/2 triangular phase gratings is about 21% higher than that of dual rectangular phase gratings. Under polychromatic illumination, the fringe visibility of dual 5π/2 triangular phase gratings is at least 23% higher than that of dual rectangular phase gratings. Under polychromatic illumination, the greater the deviation of X-ray average energy from the grating design energy, the greater the decrease of maximum fringe visibility of the dual phase grating interferometer is. In addition, with the increase of the focal size of X-ray source, the maximum fringe visibility of the dual phase grating interferometer decreases, under polychromatic illumination. We hope that those results can be used as guidelines for designing and optimizing X-ray interferometer using dual triangular phase gratings.

Phase imaging of irradiated foils at the OMEGA EP facility using phase-stepping X-ray Talbot–Lau deflectometry

Abstract Diagnosing the evolution of laser-generated high energy density (HED) systems is fundamental to develop a correct understanding of the behavior of matter under extreme conditions. Talbot–Lau interferometry constitutes a promising tool, since it permits simultaneous single-shot X-ray radiography and phase-contrast imaging of dense plasmas. We present the results of an experiment at OMEGA EP that aims to probe the ablation front of a laser-irradiated foil using a Talbot–Lau X-ray interferometer. A polystyrene (CH) foil was irradiated by a laser of 133 J, 1 ns and probed with 8 keV laser-produced backlighter radiation from Cu foils driven by a short-pulse laser (153 J, 11 ps). The ablation front interferograms were processed in combination with a set of reference images obtained ex situ using phase-stepping. We managed to obtain attenuation and phase-shift images of a laser-irradiated foil for electron densities above ${10}^{22}\;{\mathrm{cm}}^{-3}$ . These results showcase the capabilities of Talbot–Lau X-ray diagnostic methods to diagnose HED laser-generated plasmas through high-resolution imaging.

Three-dimensional model of a split-crystal X-ray and neutron interferometer

The observation of neutron interference using a crystal interferometer having a separate analyser opens the way to the construction and operation of interferometers with vast arm separation and length. Setting the design specifications requires a three-dimensional dynamical theory model of their operation. This paper develops the required three-dimensional mathematical framework, which also comprises coherent and incoherent illuminations; it is applied to study the visibility of the interference fringes.

Signal recovery of a Fabry–Pérot interferometric x-ray pulse detector based on the RadOptic effect

The signal recovery of a Fabry–Pérot interferometric x-ray pulse detector based on the RadOptic effect in the non-limiting case was investigated in this research. A Fe-doped InP with an invariant excess carrier recombination mechanism was used as the interference cavity material to achieve a constant temporal instrumental response function (tIRF). A linear and time-invariant detection system described by the convolution of the time-varying x-ray pulse and the constant tIRF was established based on the transient refractive index variation model determined by the three effects of band filling, band shrinkage, and free-carrier absorption. For the non-limiting case, the accumulation of excess carriers enhanced the sensitivity but altered the fluctuations of the real x-ray pulse. To realistically reconstruct the x-ray pulse, two-photon absorption of the infrared ultrashort pulse was used to simulate the ultrashort x-ray excitation to obtain the tIRF. Finally, using the conjugate gradient method, the original signal recorded by the detection system was deconvoluted to recover the signal. The success of signal recovery in the non-limiting case provided the basis for the development of detectors with adjustable sensitivity controlled by carrier lifetime.

Statistical optics modeling of dark-field scattering in X-ray grating interferometers: Part 2. Simulation

A grating-based Talbot-Lau X-ray interferometer provides three imaging modalities, namely attenuation, differential phase contrast, and dark field. Of these, dark-field imaging is uniquely capable of detecting and characterizing micron-scale fine structure in an object via small-angle scattering that reduces fringe visibility. In Part 1 [Opt. Express 29, 40891 (2021)10.1364/OE.447794], we formulate a statistical optics model that predicts the change in visibility, or dark-field signal, as a function of the statistical properties of the scattering object as well as its location within the interferometer. In Part 2, we demonstrate use of this model by simulating an object comprising a random collection of scattering microspheres placed in an X-ray grating interferometer designed to operate at 28 keV. The statistical optics results are validated by numerical Fourier optics simulations.

Statistical optics modeling of dark-field scattering in X-ray grating interferometers: Part 1. Theory

A grating-based Talbot-Lau X-ray interferometer provides three imaging modalities, namely attenuation, differential phase contrast, and dark field. Of these, dark-field imaging is uniquely capable of detecting and characterizing micron-scale fine structure in an object via small-angle scattering that reduces fringe visibility. Several empirical studies have been published showing the utility of this imaging modality for a wide range of applications. There also exists a more limited set of theoretical papers, based primarily on wave-optics formulations. In this two-part paper we present a comprehensive statistical optics model of the dark-field effect. In Part 1, we develop the theoretical underpinnings of the model with an emphasis on a scattering object comprising a random collection of microspheres, and in Part 2 [Opt. Express 29, 40917 (2021)10.1364/OE.447798], we provide a variety of example simulation results.

Defocused travelling fringes in a scanning triple-Laue X-ray interferometry setup.

The measurement of the silicon lattice parameter by a separate-crystal triple-Laue X-ray interferometer is a key step for the realization of the kilogram by counting atoms. Since the measurement accuracy is approaching nine significant digits, a reliable model of the interferometer operation is required to quantify or exclude systematic errors. This paper investigates both analytically and experimentally the effect of the defocus (the difference between the splitter-to-mirror and analyser-to-mirror distances) on the phase of the interference fringes and the measurement of the lattice parameter.

Fabrication of X-ray Gratings for Interferometric Imaging by Conformal Seedless Gold Electroplating.

We present a method to produce small pitch gratings for X-ray interferometric imaging applications, allowing the phase sensitivity to be increased and/or the length of the laboratory setup to be minimized. The method is based on fabrication of high aspect ratio silicon microstructures using deep reactive ion etching (Bosch technique) of dense grating arrays and followed by conformal electroplating of Au. We demonstrated that low resistivity Si substrates (<0.01 Ohm·cm) enable the metal seeding layer deposition step to be avoided, which is normally required to initiate the electroplating process. Etching conditions were optimized to realize Si recess structures with a slight bottom tapering, which ensured the void-free Au filling of the trenches. Vapor HF was used to remove the native oxide layer from the Si grating surface prior to electroplating in the cyanide-based Au electrolyte. Fabrication of Au gratings with pitch in the range 1.2–3.0 µm was successfully realized. A substantial improved aspect ratio of 45:1 for a pitch size of 1.2 µm was achieved with respect to the prior art on 4-inch wafer-based technology. The fabricated Au gratings were tested with X-ray interferometers in Talbot–Laue configuration with measured visibility of 13% at an X-ray design energy of 26 keV.

Phase-contrast and dark-field imaging for the inspection of resin-rich areas and fiber orientation in non-crimp vacuum infusion carbon-fiber-reinforced polymers

In this work, we present a multimodal approach to three-dimensionally quantify and visualize fiber orientation and resin-rich areas in carbon-fiber-reinforced polymers manufactured by vacuum infusion. Three complementary image modalities were acquired by Talbot–Lau grating interferometer (TLGI) X-ray microcomputed tomography (XCT). Compared to absorption contrast (AC), TLGI-XCT provides enhanced contrast between polymer matrix and carbon fibers at lower spatial resolutions in the form of differential phase contrast (DPC) and dark-field contrast (DFC). Consequently, relatively thin layers of resin, effectively indiscernible from image noise in AC data, are distinguishable. In addition to the assessment of fiber orientation, the combination of DPC and DFC facilitates the quantification of resin-rich areas, e.g., in gaps between fiber layers or at binder yarn collimation sites. We found that resin-rich areas between fiber layers are predominantly developed in regions characterized by a pronounced curvature. In contrast, in-layer resin-rich areas are mainly caused by the collimation of fibers by binder yarn. Furthermore, void volume around two adjacent 90°-oriented fiber layers is increased by roughly 20% compared to a random distribution over the whole specimen.

High sensitivity X-ray phase contrast imaging by laboratory grating-based interferometry at high Talbot order geometry.

X-ray phase contrast imaging is a powerful analysis technique for materials science and biomedicine. Here, we report on laboratory grating-based X-ray interferometry employing a microfocus X-ray source and a high Talbot order (35th) asymmetric geometry to achieve high angular sensitivity and high spatial resolution X-ray phase contrast imaging in a compact system (total length <1 m). The detection of very small refractive angles (∼50 nrad) at an interferometer design energy of 19 keV was enabled by combining small period X-ray gratings (1.0, 1.5 and 3.0 µm) and a single-photon counting X-ray detector (75 µm pixel size). The performance of the X-ray interferometer was fully characterized in terms of angular sensitivity and spatial resolution. Finally, the potential of laboratory X-ray phase contrast for biomedical imaging is demonstrated by obtaining high resolution X-ray phase tomographies of a mouse embryo embedded in solid paraffin and a formalin-fixed full-thickness sample of human left ventricle in water with a spatial resolution of 21.5 µm.

INVESTIGATING THE IMPACT OF AN EXTERNAL INFLUENCE ON THE DYNAMIC BEHAVIOR OF DISLOCATIONS IN SILICON CRYSTALS

The results of studying of the influence of a constant magnetic field on the dynamic behavior of dislocations in the crystalline block of an interferometer subsequently subjected to uniaxial mechanical tensile stress along the crystallographic axis of silicon are presented. The periodicity of the dilatation moire image after these influences, the average means free path of a dislocation in a crystal (block), the amount of slip, the average density of dislocations along the slip line, the relative deformation, and Young's modulus are calculated. To study the effect of a stable magnetic field on the dynamic behavior of dislocations in silicon crystals, a special three-block X-ray interferometer was fabricated in one of the blocks, and dislocations were introduced using the technique proposed by us. The experiments were carried out for various values of the magnetic field induction and mechanical stress. It is shown that the sequential action of these external influences leads to an increase in the starting stress, a decrease in the velocity of dislocation movement, a delay in the onset of dislocation movement, and the appearance of a hardening phenomenon. Experiments show that the displacement mobility characteristics are especially sensitive when the modulus of the magnetic induction vector reaches a certain threshold value for a given sample. It was shown that, in a sample containing silicon dislocations, the magnetic memory that appears after storage in a magnetic field is short-lived. It is found that the speed of movement of a dislocation in a magnetic field processed by a magnetic field, "then" subjected to mechanical stress (stretching), changes, but in practice the energy of its activation does not change. A theoretical analysis of the above experimental results is carried out, their scientific substantiation is given, all the factors associated with the phenomena observed in experiments are revealed.