Sample-detector Distance Research Articles

Design and implementation of a sample environment for in situ moisture-dependent neutron dark-field imaging experiments

We present the design and construction of a custom neutron-transparent sample environment for in situ moisture-dependent neutron dark-field imaging (NDFI) experiments for the imaging facilities at the Paul Scherrer Institute (PSI), Villigen, Switzerland. This simple setup, combined with a moisture generator, features a continuous flow system to ensure a constant homogeneous flow of humid air to manipulate the sample’s moisture conditions at room temperature. To facilitate neutron dark-field imaging measurements, the chamber has a slim design to maximize the sample-detector distance scanning range. The chamber can maintain static or dynamic relative humidity conditions, allowing for humidity cycles. Beyond moisture-dependent studies, the system’s versatility allows its utilization in any type of gas stream-dependent study. This technical note details the engineering considerations, construction process, and validation of this sample environment.

Neutron transmission imaging system with a superconducting kinetic inductance detector

Abstract We optimized the design and operating conditions of our superconducting neutron detector to improve spatial resolution. We obtained the best spatial resolution of 10 μm when a Gd Siemens star pattern was mounted in close contact with the detector. Although there is a trade-off between a spatial resolution and an easiness of replacing samples, we built our superconducting neutron imaging system for measuring in both the room-temperature samples with a proper collimation ratio L/D for achieving a reasonable spatial resolution and a cryogenic temperature with the best spatial resolution for certain purposes. In this study, we obtained neutron transmission images of various samples when they were cooled down with the superconducting neutron detector. We compared the effect of a different sample-detector distance on a spatial resolution when the samples were placed either at cryogenic temperature or at room temperature. We also confirmed that our CB-KID sensor was able to observe the neutron transmission coefficient over wider energies of pulsed neutrons. We found the appearance of clear Bragg dips by the measurements of natural FeS2 single crystals and succeeded in mapping the distribution of differently-oriented crystals by choosing several Bragg dips of the FeS2 crystals to compose the transmission images.

An autofocusing strategy based on dichotomy for fast correcting the axial distance error of ptychography

In ptychography, the precise axial distance between the sample and the detector is of vital importance to retrieve the tested object with high quality, but the axial distance error cannot be entirely eliminated in the practical experiments. An autofocusing strategy based on dichotomy is proposed to rapidly correct the axial distance error. In this strategy, the total variation function that is valid for both amplitude- and phase-modulating specimens is applied to determine whether the current distance is smaller or larger than the true distance. Further, the dichotomy is used to exponentially shrink the step-size of the correction by iterative computations, which means that for the early iterations large modified step-size is used and for later iterations only small step-size is considered. Therefore, the dichotomy is beneficial to quickly confirm the accurate axial distance with few computations. Simulations and experiments are conducted to demonstrate that our proposed strategy, based on the extended ptychographic iterative engine (ePIE), is capable of calibrating the sample–detector distance with high accuracy and efficiency.

A practical and general methodology for efficiency calibration of coaxial Ge detectors

The correct determination of artificial and natural radionuclides like 152Eu, 137, 134Cs, 60, 57Co, etc., and 234, 228Th, 228, 226Ra, 210Pb and 40K, respectively, is essential for many environmental science fields. For this, a general function was obtained for the full-energy peak efficiency (FEPE) by gamma-ray spectrometry using coaxial Ge detectors. Then, the experimental FEPE values, obtained fixing the energy, Eγ, were fitted varying the thickness, h, of cylindrical standards. The parameters resulted from these fittings were fitted, in turn, versus Eγ, obtaining a general efficiency function, εc (Eγ, h). εc (Eγ, h) was validated, obtaining very good zscore, except for Eγ affected by TCS effects. Consequently, a practical and general method was developed, recalibrating the detector by varying the sample-detector distance, d. εc (Eγ, h, d) was obtained, achieving very good zscore. Furthermore, this practical method was also employed to correct high self-absorptions and high dead times.

Mixed Metal oxide Nanofillers Introduced Poly (vinyl alcohol) based Light-Diffusing Nanocomposites: An Optical Study

Mechanically flexible optical diffusers are of significant interest for those optical applications, which demand homogenization of emitted light. These functional materials operate by avoiding the occurrence of otherwise undesirable locally concentrated light. Herein, we report the development and performance evaluation of one such optical diffuser, which was realized using the polymer nanocomposite (PNC) approach. Where, poly (vinyl alcohol) (PVA), acts as the carrier for the light diffusion system, while Mg0.2Ce0.4O nanoparticles serve the role of light-diffusing filler. Further, the success of PNC formation was ascertained from the microstructural changes recorded using powder X-ray diffraction (P-XRD) studies. While Mg0.2Ce0.4O nanofiller induced changes in surface morphological characteristics of PVA were established using scanning electron microscopy (SEM) studies. While, an electronic spectral study was engaged to establish the optical behaviors of PVA/Mg0.2Ce0.4O NC thick films. Finally, a laser source and a digital camera supported with image processing tools were used to probe the light-diffusing abilities of PVA/Mg0.2Ce0.4O NCs. Going forward, the effect of refractive index (RI) difference and sample-detector separation distance on optical properties of light-diffusing films were also evaluated. And the abilities of light-diffusing PNCs to improve the brightness uniformity of white LEDs were also ascertained. The experimental fallouts support that, the mechanically flexible PVA/Mg0.2Ce0.4O NCs show appreciable light-diffusing abilities. Such PNCs showing appreciable improvement in brightness uniformities of emanating light are of considerable interest in artificial lightings and display devices.

Review and experimental verification of x-ray dark-field signal interpretations with respect to quantitative isotropic and anisotropic dark-field computed tomography

Talbot(-Lau) interferometric x-ray and neutron dark-field imaging has, over the past decade, gained substantial interest for its ability to provide insights into a sample’s microstructure below the imaging resolution by means of ultra small angle scattering effects. Quantitative interpretations of such images depend on models of the signal origination process that relate the observable image contrast to underlying physical processes. A review of such models is given here and their relation to the wave optical derivations by Yashiro et al and Lynch et al as well as to small angle scattering is discussed. Fresnel scaling is introduced to explain the characteristic distance dependence observed in cone beam geometries. Moreover, a model describing the anisotropic signals of fibrous objects is derived. The Yashiro-Lynch model is experimentally verified both in radiographic and tomographic imaging in a monochromatic synchrotron setting, considering both the effects of material and positional dependence of the resulting dark-field contrast. The effect of varying sample–detector distance on the dark-field signal is shown to be non-negligible for tomographic imaging, yet can be largely compensated for by symmetric acquisition trajectories. The derived orientation dependence of the dark-field contrast of fibrous materials both with respect to variations in autocorrelation width and scattering cross section is experimentally validated using carbon fiber reinforced rods.

Experimental design and z-score results are useful tools for optimizing instrumental neutron activation analysis procedures

In this study 2k experimental designs were used for the optimization of an instrumental neutron activation analysis method for the determination of bromine, chlorine, magnesium, manganese, potassium, sodium and vanadium in biological matrix materials. Depending on radionuclide half-lives, 23 or 24 experimental designs were used with irradiation time, sample–detector distance, counting time and sample decay time as factors. Gamma ray spectrometer, comparator mass fraction and sample mass were kept constant. Optimized irradiation and measurement conditions were established based on the experimental design results that used z-scores as response on a reference material for the various elements and experimental conditions.

On the Genesis of Artifacts in Neutron Transmission Imaging of Hydrogenous Steel Specimens.

Hydrogen-charged supermartensitic steel samples were used to systematically investigate imaging artifacts in neutron radiography. Cadmium stencils were placed around the samples to shield the scintillator from excessive neutron radiation and to investigate the influence of the backlight effect. The contribution of scattered neutrons to the total detected intensity was investigated by additionally varying the sample-detector distance and applying a functional correlation between distance and intensity. Furthermore, the influence of the surface roughness on the edge effect due to refraction was investigated.

A compact high-resolution spectrometer based on a segmented conical crystal analyzer

In this work, the design, fabrication, and evaluation of a compact, one-shot spectrometer based on a segmented conically bent crystal analyzer are described. The system is a "one-shot" wavelength dispersive spectrometer, which has a crystal analyzer with an innovative geometry. It reaches an energy resolution of around 8 eV for Mn Kα1 line, which is at least an order of magnitude better than the commonly used energy dispersive spectrometers for fluorescence, and is comparable to current wavelength dispersive spectrometers. The prototype spectrometer fabricated in this work avoids angle scans that most wavelength dispersive spectrometers require, has the advantage of a sample-detector distance of only 146 mm, and allows for the simultaneous measurement of approximately a 2 keV window. This system is suitable to be used at synchrotron radiation facilities and free electron lasers, and it can even be adapted to an x-ray tube in any conventional x-ray laboratory.

ZPIE: an autofocusing algorithm for ptychography.

An autofocusing algorithm for ptychography is proposed. The method optimizes a sharpness metric that would be observed in a differential interference microscope and is valid for both amplitude and phase modulating specimens. We experimentally demonstrate that the algorithm, based on the extended ptychographic iterative engine (ePIE), calibrates the sample-detector distance with an accuracy within the depth of field of the ptychographic microscope. We show that the method can be used to determine slice separation in multislice ptychography, provided there are isolated regions on each slice of the specimen that do not axially overlap.

Simulation of small-angle X-ray scattering data of biological macromolecules in solution.

This article presents IMSIM, an application to simulate two-dimensional small-angle X-ray scattering patterns and, further, one-dimensional profiles from biological macromolecules in solution. IMSIM implements a statistical approach yielding two-dimensional images in TIFF, CBF or EDF format, which may be readily processed by existing data-analysis pipelines. Intensities and error estimates of one-dimensional patterns obtained from the radial average of the two-dimensional images exhibit the same statistical properties as observed with actual experimental data. With initial input on an absolute scale, [cm-1]/c[mg ml-1], the simulated data frames may also be scaled to absolute scale such that the forward scattering after subtraction of the background is proportional to the molecular weight of the solute. The effects of changes of concentration, exposure time, flux, wavelength, sample-detector distance, detector dimensions, pixel size, and the mask as well as incident beam position can be considered for the simulation. The simulated data may be used in method development, for educational purposes, and also to determine the most suitable beamline setup for a project prior to the application and use of the actual beamtime. IMSIM is available as part of the ATSAS software package (3.0.0) and is freely available for academic use (http://www.embl-hamburg.de/biosaxs/download.html).

Radon Off-Gassing From Military Artifacts.

Military historical artifacts found in museum displays and storage locations were analyzed for their Ra and Rn progeny activities to determine the fraction of Rn lost to the environment. Gamma-ray spectroscopy using high-purity germanium detectors was used to determine Ra activity and infer Rn activity based on Pb and Bi. Analyses were conducted without affecting the structural integrity of the artifacts. Ra was measured directly after correction for solid angle and finite sample-detector distance. Although Rn can be similarly analyzed, the collection in charcoal of Rn off-gassed from the artifact after the establishment of secular equilibrium was preferable. Rn off-gassing rates vary greatly between the six devices studied, with a maximum off-gassing rate of 1,850 ± 50 Bq h. Large variations in off-gassing rate were also observed between an additional 30 nominally identical dials, with a mean and standard deviation of 7.7 ± 7.1 Bq h. The work is not predictive of airborne Rn activity within museums, where building size and ventilation are significant and unique to each location. However, the significant off-gassing rates and their large variation suggest that Rn activities may be elevated in enclosed locations, such as aircraft cockpits and storage facilities.

Development of a crystal collimation system for high-resolution ultra-small-angle X-ray scattering applications.

Crystal collimation offers a viable alternative to the commonly used pinhole collimation in small-angle X-ray scattering (SAXS) for specific applications requiring highest angular resolution. This scheme is not affected by the parasitic scattering and diffraction-limited beam broadening. The Darwin width of the rocking curve of the crystals mainly defines the ultimate beam divergence. For this purpose, a dispersive Si-111 crystal collimation set-up based on two well conditioned pseudo channel-cut crystals (pairs of well polished, independent parallel crystals) using a higher-order reflection (Si-333) has been developed. The gain in resolution is obtained at the expense of flux. The system has been installed at the TRUSAXS beamline ID02 (ESRF) for reducing the horizontal beam divergence in high-resolution mesurements. The precise mechanics of the system allows reproducible alignment of the Bragg condition. The high resolution achieved at a sample-detector distance of 31 m is demonstrated by ultra-small-angle X-ray scattering measurements on a model system consisting of micrometre-sized polystyrene latex particles with low polydispersity.

A multipurpose instrument for time-resolved ultra-small-angle and coherent X-ray scattering.

This article presents the main technical features and performance of the upgraded beamline ID02 at the ESRF. The beamline combines different small-angle X-ray scattering techniques in one unique instrument, enabling static and kinetic investigations from ångström to micrometre size scales and time resolution down to the sub-millisecond range. The main component of the instrument is an evacuated detector tube of length 34 m and diameter 2 m. Several different detectors are housed inside a motorized wagon that travels along a rail system, allowing an automated change of the sample-detector distance from about 1 to 31 m as well as selection of the desired detector. For optional combined wide-angle scattering measurements, a wide-angle detector is installed at the entrance cone of the tube. A scattering vector (of magnitude q) range of 0.002 ≤ q ≤ 50 nm-1 is covered with two sample-detector distances and a single-beam setting for an X-ray wavelength of 1 Å. In the high-resolution mode, two-dimensional ultra-small-angle X-ray scattering patterns down to q < 0.001 nm-1 can be recorded, and the resulting one-dimensional profiles have superior quality as compared to those measured with an optimized Bonse-Hart instrument. In the highest-resolution mode, the beam is nearly coherent, thereby permitting multispeckle ultra-small-angle X-ray photon correlation spectroscopy measurements. The main applications of the instrument include the elucidation of static and transient hierarchical structures, and nonequilibrium dynamics in soft matter and biophysical systems.

Scalable, large area compound array refractive lens for hard X-rays

We demonstrate the fabrication of a 2D Compound Array Refractive Lens (CARL) for multi-contrast X-ray imaging. The CARL consists of six stacked polyimide foils with each displaying a 2D array of lenses with a 65 μm pitch aiming for a sensitivity on sub-micrometer structures with a (few-)micrometer resolution in sensing through phase and scattering contrast at multiple keV. The parabolic lenses are formed by indents in the foils by a paraboloid needle. The ability for fast single-exposure multi-contrast imaging is demonstrated by filming the kinetics of pulsed laser ablation in liquid. The three contrast channels, absorption, differential phase, and scattering, are imaged with a time resolution of 25 μs. By changing the sample-detector distance, it is possible to distinguish between nanoparticles and microbubbles.

PITSI: The neutron powder diffractometer for transition in structure investigations at the SAFARI-1 research reactor

The high-performance neutron powder diffraction instrument, PITSI, is located at the SAFARI-1 research reactor in South Africa. It supports both low and high temperature sample environments to facilitate in-situ parametric studies of crystallographic and magnetic phenomena covering the temperature range 1.5–1800 K. This facility has recently undergone a substantial modernization program in which all aspects of the beam delivery, conditioning and instrumentation have been upgraded. The primary neutron beam delivery system was optimised using Monte Carlo methods. Fast neutron and gamma radiation levels emanating from the radial beamline are suppressed within the biological shielding through the use of a vertical input-aperture and a 160 mm length sapphire filter located in the primary beam channel. Their use in conjunction with a vertically focussed monochromator has been found to minimally influence the useful thermal neutron flux component. Resolution and intensity optimization are achieved by having both the horizontal and vertical focuses of the monochromator variable. A resolution of Δd/d = ∼3 × 10−3 is achieved at a sample-detector distance of 1600 mm. The data acquisition and control system is standardised on the SINQ Instrument Control Software. In-house data reduction software enables flat field correction, geometric correction, vertical integration, normalization, data cropping and frame stitching.

Noise robustness of a combined phase retrieval and reconstruction method for phase-contrast tomography.

Classical reconstruction methods for phase-contrast tomography consist of two stages: phase retrieval and tomographic reconstruction. A novel algebraic method combining the two was suggested by Kostenko et al. [Opt. Express21, 12185 (2013)OPEXFF1094-408710.1364/OE.21.012185], and preliminary results demonstrated improved reconstruction compared with a given two-stage method. Using simulated free-space propagation experiments with a single sample-detector distance, we thoroughly compare the novel method with the two-stage method to address limitations of the preliminary results. We demonstrate that the novel method is substantially more robust toward noise; our simulations point to a possible reduction in counting times by an order of magnitude.

Traceable GISAXS measurements for pitch determination of a 25 nm self-assembled polymer grating

The feature sizes of only a few nanometres in modern nanotechnology and next-generation microelectronics continually increase the demand for suitable nanometrology tools. Grazing-incidence small-angle X-ray scattering (GISAXS) is a versatile technique to measure lateral and vertical sizes in the nanometre range, but the traceability of the obtained parameters, which is a prerequisite for any metrological measurement, has not been demonstrated so far. In this work, the first traceable GISAXS measurements, demonstrated with a self-assembled block copolymer grating structure with a nominal pitch of 25 nm, are reported. The different uncertainty contributions to the obtained pitch value of 24.83 (9) nm are discussed individually. The main uncertainty contribution results from the sample–detector distance and the pixel size measurement, whereas the intrinsic asymmetry of the scattering features is of minor relevance for the investigated grating structure. The uncertainty analysis provides a basis for the evaluation of the uncertainty of GISAXS data in a more general context, for example in numerical data modeling.

Time-Resolved X-Ray Stress Analysis in Multilayered Thin Films during Continuous Loading: Use of 2D Remote Detection

Synchrotron X-ray diffraction is a powerful tool to analyse the mechanical behavior of multiphase materials due to its selectivity. Simultaneous stress analysis of both phases of a W/Cu thin multilayer has been performed during a continuous biaxial loading on DiffAbs beamline at SOLEIL synchrotron (France). The use of a 2D detector with a large sample-detector distance is shown to give relatively accurate applied stress analysis even if only a small part of the usual ψ range of the sin2ψ method is considered. The results show the failure of the thin film multilayer while the W components are still under a strong compressive stress state of-3 GPa. It is concluded that the mechanical behavior is in fact mainly governed by the residual stress state.

Time-lapse X-ray phase-contrast microtomography for in vivo imaging and analysis of morphogenesis

X-ray phase-contrast microtomography (XPCμT) is a label-free, high-resolution imaging modality for analyzing early development of vertebrate embryos in vivo by using time-lapse sequences of 3D volumes. Here we provide a detailed protocol for applying this technique to study gastrulation in Xenopus laevis (African clawed frog) embryos. In contrast to μMRI, XPCμT images optically opaque embryos with subminute temporal and micrometer-range spatial resolution. We describe sample preparation, culture and suspension of embryos, tomographic imaging with a typical duration of 2 h (gastrulation and neurulation stages), intricacies of image pre-processing, phase retrieval, tomographic reconstruction, segmentation and motion analysis. Moreover, we briefly discuss our present understanding of X-ray dose effects (heat load and radiolysis), and we outline how to optimize the experimental configuration with respect to X-ray energy, photon flux density, sample-detector distance, exposure time per tomographic projection, numbers of projections and time-lapse intervals. The protocol requires an interdisciplinary effort of developmental biologists for sample preparation and data interpretation, X-ray physicists for planning and performing the experiment and applied mathematicians/computer scientists/physicists for data processing and analysis. Sample preparation requires 9-48 h, depending on the stage of development to be studied. Data acquisition takes 2-3 h per tomographic time-lapse sequence. Data processing and analysis requires a further 2 weeks, depending on the availability of computing power and the amount of detail required to address a given scientific problem.