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The Bragg-edge neutron transmission imaging method can quantitatively visualize various types of crystalline microstructural information inside a bulk material over a large visualization field area. In this study, we investigated and improved both the experimental method and the data analysis method for the evaluation of crystalline phase volume fraction in steel composed of ferrite/martensite and austenite. For wavelength-resolved neutron transmission imaging experiments, we confirmed that accurate measurement of neutron transmission intensities was crucial. Therefore, the background neutrons scattered from a sample must be reduced. Simultaneously, we confirmed that a neutron wavelength resolution of approximately 1% was required. For the data analysis of the measured Bragg-edge neutron transmission spectrum, we used double March-Dollase orientation distribution functions for each crystalline phase to achieve effective spectrum correction of the crystallographic texture effect. As a result, this data analysis method allows improved evaluation of the crystalline phase volume fraction, compared with the use of a single March-Dollase function for each phase.

A 3He spin filter is a useful device for polarizing a neutron beam. We are developing the 3He spin filters for users of the material and life science facility of the Japan Proton Accelerator Research Complex (J‑PARC). An in situ SEOP system with a 3He polarization evaluation system using nuclear magnetic resonance (NMR) method of adiabatic fast passage and electron paramagnetic resonance (EPR) was developed. We conducted an experiment on the neutron beam line BL10 (NOBORU) of J-PARC to confirm the consistency of 3He polarization, estimated using the neutron transmission, NMR and EPR. The polarization of 3He, evaluated using the different methods, was consistent and the evaluation system operated normally for about 6 h.

Energy-resolved neutron imaging is employed for in-situ measurements of dopant transport in a simple experiment performed before the crystal growth of the scintillator BaBrCl:5%Eu via a vertical gradient freeze technique. During a stabilization period preceding growth, we observed the diffusion of Eu from the solid phase into the melt over a period of approximately 4 hours. Comparing the measured centerline concentration profile with a mathematical model for the system, we estimate the solid-state diffusivity of Eu in BaBrCl as D 1 = 1.9 × 10 − 10 m2/s and an upper limit for the liquid-phase diffusivity of Eu in the melt as D 2 * = 2.5 × 10 − 10 m2/s, at temperatures near the melting point. We compare this experiment, where diffusion is driven by a concentration discontinuity arising from segregation, to the classical diffusion couple technique. Suggestions are offered on how this segregation-driven couple might be improved as a tool for measuring diffusion coefficients, and we draw attention to the great promise of neutron imaging for in-situ measurements of the distribution of elements, with sufficiently high neutron attenuation coefficients, in difficult environments.

The effect of melt convection on the phase separation structures in undercooled Cu Co alloys was investigated using the electromagnetic levitation technique, where the melt convection was controlled by applying a static magnetic field. The three-dimensional phase separation structures of the solidified Cu Co alloys were first observed using neutron computed tomography. A large number of small spherical Co-rich phases were dispersed in the Cu-rich phase matrix when the static magnetic field was relatively small. In contrast, several coalesced Co-rich phases, which were elongated along the direction of the static magnetic field, appeared in the higher strength of static magnetic field.

Neutron radiography is regarded as complementary to X-ray radiography in terms of transmittance through materials, but its spatial resolution is still insufficient. In order to achieve higher resolution in neutron imaging, several approaches have been adopted, such as optical magnification and event centroiding. In this paper, the authors focused on modification of the scintillator. A Gd3Al2Ga3O12:Ce single-crystal scintillator was applied to neutron radiography for the first time and a spatial resolution of 10.5 μm was achieved. The results indicate that this material can be a powerful candidate for a new neutron scintillator providing a resolution in micrometer order by optimizing the optical system and increasing the scintillator luminosity.

Boron carbide is used as a neutron-absorbing material in Fukushima-Daiichi Nuclear Power Station (1F), producing borides that are twice as hard as oxides (such as UO2 and ZrO2). The high neutron absorption of boron affects the evaluation of re-criticality during the process of debris retrieval. Therefore, it is important not only to determine the presence of boron but also to investigate the distribution of boron inside the material in a non-destructive manner during decommissioning. To address the uncertainties in the core material relocation behavior of boiling water reactor (BWR) during a severe accident (SA), solidified melt specimens of a simulated fuel assembly were prepared by plasma heating. If core material melting and relocation (CMMR) specimens can be used to estimate the B distribution in 1F Unit-3, that will provide valuable information in the decommissioning of 1F. To address this, the authors focused on the energy-resolved neutron-imaging system, RADEN, which utilizes a wide energy range, from meV to keV. This is an innovative three-dimensional analysis technology for boride distribution that affects the evaluation of hardness and re-criticality. In the calibration standard samples (ZrxB1-x and FexB1-x), there was a good correlation between boron concentration and the energy-dependence of the cross sections of cold and epithermal neutrons. In the CMMR specimens, boron distribution was confirmed from the contrast difference between cold and epithermal neutrons. In the future, the results of calibration standard samples will be applied to the results of CMMR specimens. With this method, three-dimensional boron distribution will be measured, and the understanding of boride distribution 1F Unit-3 will be improved, which may be reflected in an improved SA code.

Solidification process of lead–bismuth eutectic (LBE) is one of the key phenomena to prevent flow channel blockage accident in an LBE-cooled accelerator-driven system. However, the solidification of liquid metal cannot be observed optically and it is difficult to detect noninvasively. In this study, the one-dimensional solidification process of the LBE was visualized by pulsed neutron transmission imaging. Neutrons have higher transmittivity to the LBE than X-ray and neutron transmission spectrum of the LBE sample can be obtained by pulsed neutron imaging technique. The solid and liquid phases of the LBE were identified during the solidification process by the presence or absence of Bragg edge in the measured neutron transmission spectrum, and the transient behavior of the solid–liquid interface could be visualized. In addition, the characteristic spatial distribution of the crystalline structure was found in Bragg-edge transmission image after the solidification.

Neutron resonance absorption imaging, being used to visualize a spatial distribution of elements and/or temperature within a sample, is one of the important applications of an intense short-pulse neutron source. Two-dimensional time-analyzer neutron detectors are indispensable to perform neutron energy dependent imaging by means of the time-of-flight technique. Some state-of-the-art time-analyzer neutron detectors have been developed for thermal or cold neutrons. However the detection efficiencies of such neutron detectors are not sufficient for neutron resonance absorption imaging which utilizes neutrons in the energy region from eV to keV. The 2012 model lithium-6 time-analyzer neutron detector (LiTA12) system, based on a lithium glass scintillator and multi-anode photomultiplier tube, has the highest neutron efficiency among the detectors for pulsed neutron imaging together with the flexibility to tune the efficiency by changing the thickness of the lithium glass. The authors estimated performances of the detector at resonance neutron energies finding that 0.7 mm width line pairs made by 3 μm thick gold could be resolved at 4.9 eV and the maximum count rate of 8 Mcps was achieved at 1 keV.

We are developing practical material observation methods using neutron imaging at J-PARC Materials and Life Science Experimental Facility (MLF). Neutron Bragg-edge transmission (BET) imaging, one of the energy-resolved neutron imaging methods, makes it possible to quantitatively visualize the two-dimensional distribution of physical properties within a sample. Here, we report two application examples. First, feasibility of measuring the temperature distribution of a copper rod through the thermal expansion of the lattice constant using BET spectral analysis was studied. Second, visualization of the texture variation and the strain distribution of a bent steel plate through the 2D-BET imaging method were performed. The obtained results for both experiments were compared with those obtained by the neutron diffraction (ND) method.

In this paper, we have studied an additively manufactured metallic component, intended for ultra-high vacuum application, the exit-snout of the MACHINA transportable proton accelerator beam-line. Metal additive manufacturing components can exhibit heterogeneous and anisotropic microstructures. Two non-destructive imaging techniques, X-ray computed tomography and Neutron Tomography, were employed to examine its microstructure. They unveiled the presence of porosity and channels, the size and composition of grains and intergranular precipitates, and the general behavior of the spatial distribution of the solidification lines. While X-ray computed tomography evidenced qualitative details about the surface roughness and internal defects, neutron tomography showed excellent ability in imaging the spatial density distribution within the component. The anisotropy of the density was attributed to the material building orientation during the 3D printing process. Density variations suggest the possibility of defect pathways, which could affect high vacuum performances. In addition, these results highlight the importance of considering building orientation in the design for additive manufacturing for UHV applications. Graphical Abstract

This study is the first report on liquid water and ice imaging conducted at a pulsed spallation neutron source facility. Neutron imaging can be utilised to visualise the water distribution inside polymer electrolyte fuel cells (PEFCs). Particularly, energy-resolved neutron imaging is a methodology capable of distinguishing between liquid water and ice, and is effective for investigating ice formation in PEFCs operating in a subfreezing environment. The distinction principle is based on the fact that the cross sections of liquid water and ice differ from each other at low neutron energies. In order to quantitatively observe transient freezing and thawing phenomena in a multiphase mixture (gas/liquid/solid) within real PEFCs with high spatial resolution, a pulsed neutron beam with both high intensity and wide energy range is most appropriate. In the validation study of the present work, we used water sealed in narrow capillary tubes to simulate the flow channels of a PEFC, and a pulsed neutron beam was applied to distinguish ice, liquid water and super-cooled water, and to clarify freezing and thawing phenomena of the water within the capillary tubes. Moreover, we have enabled the observation of liquid water/ice distributions in a large field of view (300 mm × 300 mm) by manufacturing a sub-zero environment chamber that can be cooled down to −30 °C, as a step towards in situ visualisation of full-size fuel cells.

A time-of-flight Bragg-edge neutron transmission imaging was used to investigate the microstructure and strain distributions in a gear hardened by a newly developed two-step induction-heating method: precursor (Sample 1) and final product (Sample 2). The edge-position and edge-broadening were determined and mapped with high resolution, which enabled us to confirm the two-dimensional distributions of the microstructure and residual strain. A deep hardened layer was made for Sample 1 in which martensite was formed on the entire teeth and the outer peripheral portion of the gear body. Sample 2 was subjected to double induction-hardening, where a tempered martensite was formed as the thermal refined microstructure between a fine-grained martensite at the tooth surface and a ferrite-pearlite microstructure at the core. The relationship between edge-broadening and the Vickers hardness described by a linear equation was employed to derive the elastic residual strain. The residual strain map for Sample 2 revealed that a steep compressive strain was introduced into the fine-grained martensite at the tooth surface by the super rapid induction-heating and quenching process. The reversal of tension was speculated to occur below 2 mm from the tooth tip, and the strain was almost zero in the core region.

Energy resolved neutron transmission techniques can provide high-resolution images of strain within polycrystalline samples allowing the study of residual strain and stress in engineered components. Strain is estimated from such data by analysing features known as Bragg-edges for which several methods exist. It is important for these methods to provide both accurate estimates of strain and an accurate quantification the associated uncertainty. Our contribution is twofold. First, we present a numerical simulation analysis of these existing methods, which shows that the most accurate estimates of strain are provided by a method that provides inaccurate estimates of certainty. Second, a novel Bayesian non-parametric method for estimating strain from Bragg-edges is presented. The numerical simulation analysis indicates that this method provides both competitive estimates of strain and accurate quantification of certainty, two demonstrations on experimental data are then presented.

A new mapping procedure for polycrystals using neutron Bragg-dip transmission is presented. This is expected to be useful as a new materials characterization tool which can simultaneously map the crystallographic direction of grains parallel to the incident beam. The method potentially has a higher spatial resolution than neutron diffraction imaging. As a demonstration, a Bragg-dip neutron transmission experiment was conducted at J-PARC on beamline MLF BL10 NOBORU. A large-grained Si–steel plate was used. Since this specimen included multiple grains along the neutron beam transmission path, it was a challenging task for existing methods to analyse the direction of the crystal lattice of each grain. A new data-analysis method for Bragg-dip transmission measurements was developed based on database matching. As a result, the number of grains and their crystallographic direction along the neutron transmission path have been determined.

Microstructures produced by Additive Manufacturing (AM) techniques determine many characteristics of components produced by this particular manufacturing technique. Residual stress and texture are among those characteristics, which need to be optimized to meet dimensional and strength requirements. Post-build heat treatments are necessary to relief residual stresses, homogenize the microstructure and to develop the necessary microstructures (precipitation or solution hardening) for strength. Our focus in this study is the measurement of residual stresses during a vacuum stress relief (VSR) heat treatment. We employ the energy-resolved neutron imaging to investigate, in-situ, the uniformity of the as-built texture and to map the residual strain distributions within samples of Inconel 625 (IN625). The samples used in this study were printed using the powder-bed metal laser melting additive manufacturing technique. Strain and texture variations were measured at room temperature for the as-built samples as well as their changes during stress relief annealing at 700 °C and 875 °C in a vacuum furnace. The uniformity of crystalline plane distribution, from which texture can be inferred, was imaged with sub-mm spatial resolution for the entire sample area exceeding several square centimeters. Despite the limited accuracy of in-situ lattice strain reconstruction during sample annealing, the results indicate that most of the strain relaxation occurs at 700 °C within the first 2–3 h. Relaxation of the strain at 875 °C happened at a much faster rate. In addition, energy-resolved neutron imaging demonstrates the possibility to correlate the uniformity of grain orientation and the degree of texture variations with printing parameters, in particular the laser translation speed. Simulations of the AM build process were carried out to predict the residual stress distributions within the samples as a function of the build process parameters. Comparisons of the simulation results to the room temperature experimental measurements show good agreements when the simulation data are averaged over the volume of the part confirming the usefulness of the experiments for validating simulation results. The neutron imaging technique described in this study can be helpful for the evaluation of bulk crystallographic characteristics in AM printed materials and can be used as a guide for developing the heat treatment cycle and for validations of VSR simulation results.

The reliability of neutron resonance thermometry was discussed based on measurements of neutrons transmitted through tantalum (0.1 mm thick) and tungsten (1 mm thick) indicators at 26, 96, 189, and 285 degrees Celsius using the energy-resolved neutron imaging system, RADEN, at the Japan Proton Accelerator Complex (J-PARC). The intensity of transmitted neutrons at the sides of resonance dips were found to decrease with increasing temperature. Sensitivity coefficients to convert this decrease to temperature were derived, and two-dimensional distributions of the decreasing rates, being proportional to the temperature distribution, were obtained. The reliability of estimated temperature was calculated as a function of temporal and spatial resolution assuming that the dominant factor of the reliability was the uncertainty in the neutron counts. The authors set a target of neutron resonance thermometry for practical applications, and found a required efficiency of the neutron detector for resonance thermometry.

Pulsed neutron transmission spectroscopy was applied to clarify a phase change phenomena of lead-bismuth eutectics (LBE). The melting and solidification behaviors of the LBE should be well understood to enhance the safety of an LBE-cooled accelerator driven system. In this study, the heating experiments were performed using a rectangular test section and LBE phase change process was visualized by the energy-resolved pulsed neutron imaging at BL22 RADEN facility in J-PARC and the solid/liquid interface was identified from the radiograph and Bragg edge information. The transient location of the interface was compared with measured temperature profiles and it would be useful to evaluate the LBE thermal properties., 8th International Topical Meeting on Neutron Radiography (ITMNR-8) Beijing, China, September 4-8, 2016

We have performed neutron radiography and tomography using a CCD camera-type detector for some test samples at RADEN. The current spatial resolution for neutron radiography is estimated to about 350 μm in the largest field-of-view of 300 × 300 mm2 and 100 μm in the field-of-view of 60 × 60 mm2. It is thought that the latter spatial resolution is strongly affected by the image blur in the scintillator screen. In the case of neutron tomography, the current spatial resolution is estimated to be better than 0.5 mm using an iron and aluminum test sample. Furthermore, we have performed neutron tomography for a cast aluminum product. As a result, small blowholes are found in the center of the product. This demonstrates the importance of non-destructive testing by neutron radiography and tomography for industrial products.

The influences of bending deformation and subsequent subzero treatment on the martensite transformation behaviors in a metastable austenitic alloy Fe−25 wt.% Ni−0.4 wt.% C were investigated by the time-of-flight (TOF) neutron Bragg-edge transmission (BET) imaging method. Two-dimensional (2D) maps of martensite phase volume fractions and texture variations due to residual stress and lowering the temperature of the bent samples before and after subzero treatment were obtained by Bragg-edge spectral analysis. The obtained phase volume fractions were quantitatively compared with those determined by neutron diffraction.

For the neutron phase imaging with a Talbot-Lau interferometer, we have fabricated neutron absorption gratings with a pitch of 9 μm by oblique evaporation of gadolinium. The performances of these gratings for the phase measurement were experimentally evaluated at RADEN in J-PARC, by observing the neutron transmission and the visibility of moire fringe in the interferometer. A new analysis method using the wavelength-resolved neutron transmission was also attempted to estimate the characteristics of gratings.

The RITS code is a unique and powerful tool for a whole Bragg-edge transmission spectrum fitting analysis. However, it has had two major problems. Therefore, we have proposed methods to overcome these problems. The first issue is the difference in the crystallite size values between the diffraction and the Bragg-edge analyses. We found the reason was a different definition of the crystal structure factor. It affects the crystallite size because the crystallite size is deduced from the primary extinction effect which depends on the crystal structure factor. As a result of algorithm change, crystallite sizes obtained by RITS drastically approached to crystallite sizes obtained by Rietveld analyses of diffraction data; from 155% to 110%. The second issue is correction of the effect of background neutrons scattered from a specimen. Through neutron transport simulation studies, we found that the background components consist of forward Bragg scattering, double backward Bragg scattering, and thermal diffuse scattering. RITS with the background correction function which was developed through the simulation studies could well reconstruct various simulated and experimental transmission spectra, but refined crystalline microstructural parameters were often distorted. Finally, it was recommended to reduce the background by improving experimental conditions.

Line broadening analysis was performed on the time-of-flight neutron diffraction data for the plastically bent plates of a ferritic steel and a duplex stainless steel. A Rietveld analysis program, Z-Rietveld ver. 1.0 was used to fit the anisotropically broadened patterns where the increase in Lorentzian full width at half maximum (FWHM) and the Gaussian FWHM involves information of the crystallite size and the dislocation density, respectively. The derived results were compared with those obtained by using Bragg-edge transmission spectrum analysis and electron backscatter diffraction (EBSD) observations.

This paper presents a proof-of-concept demonstration of triaxial strain tomography from Bragg-edge neutron imaging within a three-dimensional sample. Bragg-edge neutron transmission can provide high-resolution images of the average through thickness strain within a polycrystalline material. This poses an associated rich tomography problem which seeks to reconstruct the full triaxial strain field from these images. The presented demonstration is an important step towards solving this problem, and towards a technique capable of studying the residual strain and stress within engineering components. A Gaussian process based approach is used that ensures the reconstruction satisfies equilibrium and known boundary conditions. This approach is demonstrated experimentally on a non-trivial steel sample with use of the RADEN instrument at the Japan Proton Accelerator Research Complex. Validation of the reconstruction is provided by comparison with conventional strain scans from the KOWARI constant-wavelength strain diffractometer at the Australian Nuclear Science and Technology Organisation and simulations via finite element analysis.

A mapping measurement using pulsed neutron diffraction with time-of-flight method is performed on a full-shape Japanese sword made in Keicho era (1596-1615). The obtained diffraction patterns are analyzed by the Rietveld refinement and a line profile analysis. The constituent phases in the area closer to the back of the blade (ridge) are found to be ferrite and cementite, composing pearlite, while the area close to the edge is composed by martensite and austenite. The distributions of constituent phases are well explained with the distributions of dislocation density and crystallite size. The residual macroscopic stresses are estimated from the obtained lattice parameters of constituent phases. The distributions of residual macroscopic stresses in the width and thickness directions are small. The stress in the longitudinal direction is compressive at the ridge side, turns to quite large tensile at the middle part of width, then drastically decreases to be quite large compressive at the edge side of about -650 MPa. The carbon content in the area closer to the ridge side is high, about 0.9 mass%, expecting that the Japanese sword used in this study was created by the technique of maru, i.e., the use of a single type of high-carbon steel for the whole volume.

Metallic glass (MG) exhibits viscous flow behavior in the supercooled liquid (SCL) state, which is of great advantage for its net-forming process. However, the viscous workability varies strongly with the alloy system and/or composition. In this paper, we demonstrate how MG with less viscous workability such as Gd-based MG can be processed in the SCL region. Based on this understanding, high aspect ratio analyzer gratings of 9 μm pitch and ∼30 μm heights have been fabricated through an imprinting method by allowing crystallization during a rapid heating isochronal imprinting process. The analyzer gratings made of Gd-based MG have brought a breakthrough for advancing neutron phase imaging based on grating interferometer.

Neutron Bragg-edge transmission imaging makes it possible to quantitatively visualize the two-dimensional distribution of microstructure within a sample. In order to examine its application to engineering products, time-of-flight Bragg-edge transmission imaging experiments using a pulsed neutron source were performed for plastically bent plates composed of a ferritic steel and a duplex stainless steel. The non-homogeneous microstructure distributions, such as texture, crystalline size, phase volume fraction and residual elastic strain, were evaluated for the cross sections of the bent plates. The obtained results were compared with those by neutron diffraction and electron back scatter diffraction, showing that the Bragg-edge transmission imaging is powerful for engineering use.

Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 μm resolution) distribution of some microstructure properties, such as residual strain, texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. In addition, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.

Energy-resolved neutron imaging is used for a nondestructive study of bulk internal microstructure, elemental composition and distribution of voids in dissimilar metal-alloy welds of ∼10 mm thickness. All these characteristics are measured simultaneously in one experiment with a few hundred micrometre spatial resolution., A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participating alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al–steel weld is clearly resolved and could be used to optimize the welding process. A highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption.

Additive manufacturing is a promising and rapidly rising technology in metal processing. However, besides a number of key advantages the constitution of a part through a complex thermo-mechanical process implies also some severe issues with the potential of impacting the quality of products. In laser powder bed fusion (LPBF), the most applied metal additive manufacturing process, the repetitive heating and cooling cycles induce severe strains in the built material, which can have a number of adverse consequences such as deformation, cracking and decreased fatigue life that might lead to severe failure even already during processing. It has been reported recently that the application of laser shock peening (LSP) can counteract efficiently the named issues of LPBF through the introduction of beneficial compressive residual stresses in the surface regions mostly affected by tensile stresses from the manufacturing process. Here we demonstrate how lattice strains implied by LPBF and LSP can efficiently be characterized through diffraction contrast neutron imaging. Despite the spatial resolution need with regards to the significant gradients of the stress distribution and the specific microstructure, which prevent the application of more conventional methods, Bragg edge imaging succeeds to provide essential two-dimensionally spatial resolved strain maps in full field single exposure measurements.

In this study, the effects of carbon concentration and magnetic transition on the austenite lattice parameter of Fe-30Mn-xC alloys were assessed. A linear relationship was obtained between the carbon content and the lattice parameter determined by neutron diffraction and neutron Bragg-edge transmission imaging for austenitic steels bearing 0.007–1.20 mass% C. The results obtained through both methods showed good agreement. In addition, carbon partitioning was evaluated in artificially piled-up discs with different carbon contents in order to develop a new technique for advanced multi-phase steels. The analysis of asymmetry and broadening of the diffraction line profile revealed that the carbon partitioning could be determined. In addition, the Neel temperature was determined by in situ neutron diffraction upon heating and cooling with magnetic diffraction peaks and the change in the lattice parameter with temperature being monitored. The temperature dependence of the austenite lattice parameter was found to become smaller below the Neel temperature. In conclusion, the results presented herein expand the current knowledge on the properties of high Mn austenite.

Under the JST-ERATO project in progress to develop X-ray and neutron phase-imaging methods together, recent achievements have been selected and reviewed after describing the merit and the principle of the phase imaging method. For X-ray phase imaging, recent developments of four-dimensional phase tomography and phase microscopy at SPring-8, Japan are mainly presented. For neutron phase imaging, an approach in combination with the time-of-flight method developed at J-PARC, Japan is described with the description of new Gd grating fabrication.

In this study we compare conventional X-ray imaging with neutron radiography and neutron tomography of several crowned teeth and teeth with amalgam fillings. While X-ray images provide detailed information about the root area, they cannot probe anything in the area where metals are present, e.g. underneath the crown or behind the metal filling. Our results demonstrate that neutron radiography and neutron tomographic imaging can reveal the internal structure of treated teeth underneath the crown. These neutron imaging methods can be used to investigate the interaction of various fillings and crown attachment paste with the crown and the tooth itself. The integrity of tooth and fillings underneath the crown, the location of cavities and voids can be visualized in three dimensions and provide means for the improvements of dental filling and crown attachment materials and methods.

Through the use of Time-of-Flight Three Dimensional Polarimetric Neutron Tomography (ToF 3DPNT) we have for the first time successfully demonstrated a technique capable of measuring and reconstructing three dimensional magnetic field strengths and directions unobtrusively and non-destructively with the potential to probe the interior of bulk samples which is not amenable otherwise. Using a pioneering polarimetric set-up for ToF neutron instrumentation in combination with a newly developed tailored reconstruction algorithm, the magnetic field generated by a current carrying solenoid has been measured and reconstructed, thereby providing the proof-of-principle of a technique able to reveal hitherto unobtainable information on the magnetic fields in the bulk of materials and devices, due to a high degree of penetration into many materials, including metals, and the sensitivity of neutron polarisation to magnetic fields. The technique puts the potential of the ToF time structure of pulsed neutron sources to full use in order to optimise the recorded information quality and reduce measurement time., Comment: 12 pages, 4 figures

Energy-resolved neutron imaging at a pulsed source utilizes the energy-dependent neutron transmission measured via time-of-flight to extract quantitative information about the internal microstructure of an object. At the RADEN instrument at J-PARC in Japan, we use cutting-edge detectors employing micro-pattern detectors or fast Li-glass scintillators and fast, all-digital data acquisition to perform such measurements, while continuing their development toward better utilization of the intense neutron source. In particular, for the Micro-Pixel Chamber based Neutron Imaging Detector ({\mu}NID), a micro-pattern detector with a 400 {\mu}m pitch and employing 3He for neutron conversion, we have successfully improved the spatial resolution from 200 to 100 {\mu}m, increased the detection efficiency from 18 to 26% for thermal neutrons, and increased the maximum count rate from 0.4 to 1 Mcps. We are also testing a new readout element with a 215 {\mu}m pitch for further improved spatial resolution, and a {\mu}NID with boron-based neutron converter for increased rate performance., Comment: 8 pages, 5 figures; accepted to Proceedings of International Conference on Neutron Optics 2017, Nara, Japan (JPS Conference Proceedings)

Planar solid oxide electrochemical cells (SOC) are composed of at least three layers: a anode, a electrolyte and a cathode [1]. Cermet Ni-YSZ (yttria stabilized zirconia) is a material widely used for production of anodes in solid oxide fuel cells (SOFC) and cathodes in solid oxide electrolysis cells (SOEC), but also for supports. Mechanical and electrochemical performance of these layers, and thus whole cells, depends on their microstructure. One of the commonly used deposition techniques of the Ni-YSZ supports is tape-casting from a NiO-YSZ slurry, followed by sintering and reduction of NiO during the initial operation of the cell. Conditions, i.e. temperature, atmosphere and stress, applied during this procedure, determine the microstructure of the support and thereby the cell performance, therefore in-situ observation of these processes under different conditions can provide knowledge needed to optimize the SOC performance. Neutron imaging [2] is a nondestructive measurement method holding a great potential for in-situ characterization of SOC. In contrast to X-ray imaging, due to high material penetration by neutrons, it is possible not only to image real size SOC stacks, but also to perform experiments in-situ, using sample environment providing the SOC operation conditions. Here we present the results of energy resolved neutron imaging measurements applied to in-situ investigations of Ni-YSZ anode supports for SOFCs. The energy resolved neutron imaging technique is based on the measurement of neutron transmission through the sample depending on neutron energy/wavelength. In the achieved patterns, sudden changes in transmission/ attenuation – so called “Bragg edges”- occur at certain neutron wavelengths, which correspond to d-spacing values present in the investigated polycrystalline material. Thus, such Bragg edge patterns (fig.1a) contain information about elements, crystal structure, crystalline phases in a sample, texture or strain field. Bragg edge patterns can be measured both at continuous and pulsed neutron sources. In the first case, where a polychromatic continuous neutron beam is generated, Bragg edge patterns are obtained by selecting specific neutron wavelengths using monochromators and subsequent measurements of transmission for different wavelengths. In the second case, where pulses of white neutron radiation are created, neutrons with different wavelength (and velocity) reach the sample at different times. Using detectors able to record simultaneously intensity of the transmitted beam and corresponding neutron arrival time, whole Bragg edge patterns are acquired at once. This approach is called time of flight (TOF) method. We present the results of in-situ investigation of NiO reduction and re-oxidation in anode supports performed by means of energy resolved neutron imaging at both continuous (SINQ, PSI ,fig.1b) and pulsed neutron source ( ISIS, fig.1a). Figure 1a presents Bragg edge patterns recorded at ISIS around an edge corresponding to the d-spacing of NiO(200). Different patterns were measured at different times during the reduction. It is apparent, how the height of the NiO edge decreases with time. As the edge height depends on the amount of the NiO phase, it is possible to compare the reaction rate in different regions of the sample by evaluating the Bragg edge patterns for these regions. In our previous work [3] we have demonstrated by ex-situ Bragg edge neutron imaging feasibility to detect and distinguish Ni and NiO phases within the Ni-YSZ composite. Figure 1b shows the Ni and NiO phase distribution in Ni-YSZ bars after consecutive reduction and re-oxidation processes performed at a continuous neutron source. In-situ neutron imaging was performed using our custom built furnace [4]. Its design allows to meet the requirements of the equipment used at neutron imaging instruments, to achieve the required spatial resolution of images, and at the same time, to provide conditions required for conducting NiO reduction i.e. high temperature and reactive atmosphere. Since in a real SOFC, anode supports are always exposed to high thermal and mechanical stresses, progress of NiO-YSZ reduction should be investigated in samples under applied stress [5]. Therefore, our furnace is equipped with a loading system for applying stress to the sample during the reduction process. In this work, we present results of in-situ observation of the phase transition during the NiO-YSZ reduction and re-oxidation performed under different conditions: different temperatures, with and without applied stress. [1] S. Singhal, Solid State Ionics, vol. 135, no. 1–4, pp. 305–313, Nov. 2000. [2] M. Strobl et al., J. Phys.D.Appl.Phys., vol. 42, no. 24, p. 243001, Dec. 2009. [3] M. G. Makowska et al.; J. Appl. Cryst. 48, doi:10.1107/S1600576715002794, 2015. [4] M. G. Makowska et al.; submitted to RSI , 2015. [5] H. L. Frandsen et al., Conf. Proc. Eur. Fuel Cell Forum, Lucerne, Switz., 2014. Figure 1

Neutron diffractometry has been a critical tool for clarifying spin structures. In contrast, little attention has been paid to neutron transmission spectroscopy, even though they are different types of the same phenomenon. Soon, it will be possible to measure the wavelength dependence of transmissions easily using accelerator-driven neutron facilities. Therefore, we have started studying the potential of spectroscopy in magnetism, and in this paper, we report the first observation of a magnetic Bragg dip and Bragg edge in the neutron transmission spectra of a typical spin superstructure; clear antiferromagnetic Bragg dips and Bragg edges are found for a single crystal and powder of nickel oxide, respectively. The obtained results show that transmission spectroscopy is a promising tool for measurements under multi-extreme conditions and for the precise analyses of spin structures, not only in MW-class pulsed spallation source facilities but also in compact neutron source facilities.

Energy-resolved neutron imaging at a pulsed source utilizes the energy-dependent neutron transmission, measured via time-of-flight, to extract quantitative information on the internal microstructure of an object in situ. These techniques, however, are currently limited by the count-rate capability of available imaging detector systems, resulting in long measurement times and reduced spatial resolution. At RADEN, we are building on our previous detector development work to provide nearly three times improvement in rate performance of our micro-pixel chamber based neutron imaging detector $(_{\mu }$ NID) by changing from 3 He to a boron-based neutron converter and optimizing the shape for a much reduced event size and maximized detection efficiency. We are also designing a new micro-pattern readout element with an additional readout axis to facilitate clean event separation under high-rate conditions. Proof-of-principle testing at RADEN of the $_{\mu }$ NID with a flat, $1.2{\mu }m$ thick $^{10}B$ conversion layer confirmed a spatial resolution of 0.45 to 0.5 mm and indicated an improvement in rate capacity up to 22 Mcps or more. Once the boron converter is optimized for detection efficiency, this detector will help to unlock the full potential of these energyresolved neutron imaging techniques at pulsed sources.

A Li-glass scintillation detector was applied in order to test the complementary imaging with the time-of-flight (TOF) technique. Neutron and X-ray transmission measurements were performed by using a composite source system at Hokkaido University. The TOF and pulse-height spectra for the neutron and X-ray beams were obtained with samples of metal plates. For the samples, the measured transmission rates of the neutron and X-ray beams were consistent with the calculated ones.

Technological developments in high resolution time-of-flight neutron detectors have raised the prospect of tomographic reconstruction of elastic strain fields from Bragg-edge strain images. This approach holds the potential to provide a unique window into the full triaxial stress field within solid samples. While general tomographic reconstruction from these images has been shown to be ill-posed, an injective link between measurements and boundary deformations exists for systems subject to in situ applied loads in the absence of residual stress. Recent work has provided an algorithm to achieve tomographic reconstruction for this class of mechanical system. This letter details an experimental proof-of-concept for this algorithm involving the full reconstruction of a biaxial strain field within a non-trivial steel sample. This work was carried out on the RADEN energy resolved neutron imaging instrument within the Japan Proton Accelerator Research Complex, with validation through Digital Image Correlation and constant wavelength neutron strain scans.

The physical properties of polycrystalline materials depend on their microstructure, which is the nano-to-centimeter-scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study bulk samples with sizes in the cm range with a resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD)., Submitted