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Lattice misfit in nickel-based superalloys is one of the important microstructural parameters that control their mechanical properties, such as creep behaviour at high temperatures. Here, energy-resolved neutron imaging experiments are performed at a spallation neutron source to determine the spatial variation of lattice misfit on a second-generation nickel-based single-crystal superalloy specimen produced from a failed low-cycle fatigue specimen. The wavelength spectrum of the neutrons scattered by the specimen displays a large number of peaks, each corresponding to a spot in traditional Laue diffraction experiments. An analysis of the position and width of those Laue peaks in the transmission spectra allows determination of the lattice parameters of the γ and γ′ phases that compose the specimen, as well as the strain misfit and the misorientation between them. An analytical model is developed to describe the full wavelength pattern of Laue peaks arising from a specimen composed of two single crystals, and this model is used to perform least-squares refinements of the spectra measured at different positions of the specimen, with a spatial resolution of ∼500 × 500 µm. The local variations of the lattice parameter across the sample area were less than 4 mÅ for both phases, and the lattice misfit remains essentially constant at a value of 0.30 ± 0.03%, whilst the misorientation between the two phases is always smaller than 10′. By contrast, the relative misorientation between different parts of the specimen varies locally up to 1.5° on a scale of millimetres.

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.

In this work we perform a neutron Bragg edge tomography of stainless steel 316L additive manufacturing samples, one as built via standard laser powder bed fusion, and one using the novel three-dimensional (3D) laser shock peening technique. First, we consider conventional attenuation tomography of the two samples by integrating the signal for neutron wavelengths beyond the last Bragg edge, to analyze the bulk density properties of the material. This is used to map defects, such as porosities or cracks, which yield a lower density. Second, we obtain strain maps for each of the tomography projections by tracking the wavelength of the strongest Bragg edge corresponding to the {111} lattice plane family. Algebraic reconstruction techniques are used to obtain volumetric 3D maps of the strain in the bulk of the samples. It is found that not only the volume of the sample where the shock peening treatment was carried out yields a higher bulk density, but also a deep and remarkable compressive strain region. Finally, the analysis of the Bragg edge heights as a function of the projection angle is used to describe qualitatively crystallographic texture properties of the samples.

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.

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.

The capability of neutrons to penetrate materials opaque to other non-destructive techniques combined with relatively high neutron attenuation cross section for hydrogen provide unique possibilities to reveal internal distribution of water and other hydrogen-containing substances in various bulky samples. In this study we compare the accuracy of water thickness reconstruction from two types of neutron imaging experiments: neutron radiography with a white beam spectrum and energy-resolved neutron imaging. Neutron transmission spectra available at the latter modality can be used for the extraction of certain material characteristics, such as microstructure and elemental composition, usually not accessible for the analysis of images integrated over the entire neutron spectrum. Distribution of water within the sample, however, can be reconstructed from both types of neutron imaging methods. The results of present study indicate that the accuracy of water mapping appeared to be comparable within the 2%–4% error in our experiments dominated by non-optimized calibration of background signal. The accuracy of water thickness reconstruction was verified with a calibration step wedge sample for both imaging modalities. We also demonstrate the applicability of this technique for the studies of water absorptivity and porosity of ancient Roman concrete samples extracted from Cosa and Portus Traiani sites. These reconstruction methods are not only limited to quantification of water or hydrogen containing substances, but can be implemented to any other material with relatively high neutron attenuation.

For flow visualization study of quantum turbulence in superfluid $$^4$$ He, He $$_2^*$$ excimers are unique tracers which follow only normal-fluid component flow above 1 K. To generate detectable small He $$_2^*$$ clouds (clusters) required for full-space velocity field measurements, we have adopted a new method based on neutron absorption reaction of $$^3$$ He impurities in $$^4$$ He and conducted proof-of-principle experiments. Generation of the He $$_2^*$$ excimers was detected by laser-induced fluorescence using photomultiplier tubes. The fluorescence was observed to increase proportionally to the neutron flux, suggesting that a sufficient amount of He $$_2^*$$ excimers were generated by neutrons. We also estimated the number of He $$_2^*$$ excimers possibly generated by $$\gamma $$ -rays and found that the relevant contribution was less than 40%. Thus, the majority of the He $$_2^*$$ excimers was confirmed to be generated via n- $$^3$$ He absorption reactions.

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.

We have studied the effect of beam collimation on the quality of images obtained with Talbot-Lau interferometry at the RADEN beam line in the J-PARC Materials and Life Science Experimental Facility. By using four typical beam collimations of RADEN, which were determined at a position relatively far from the interferometer, the blurring of images and the average intensity and visibility of interference patterns were observed. From these data, spatial resolutions and measurement precisions of images were experimentally evaluated. The obtained characteristics on each collimation condition are useful to design and optimize a new interferometer, and perform experiments at this beam line.

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.

Residual strains in a punched electrical steel sheet increase the iron loss in the steel sheet. To accurately estimate the effect of residual strain on iron loss, the residual strain distribution in a punched electrical steel sheet should be evaluated. In this study, we demonstrated the two-dimensional imaging of the residual strain distribution in a punched electrical steel sheet using the neutron Bragg-edge transmission imaging method. To improve the accuracy of strain measurement with minimal deterioration of spatial resolution, we applied a process of superposing many specimen images. The tensile strain near the punched edge and the compressive strain inside the core were experimentally confirmed using this method. Finally, the neutron Bragg-edge imaging results and those obtained from kernel average misorientation map using electron backscattered diffraction were compared to verify the validity of the proposed method.

We are developing a neutron polarizer with polarized $^3$He gas, referred to as a $^3$He spin filter, based on the Spin Exchange Optical Pumping (SEOP) for polarized neutron scattering experiments at Materials and Life Science Experimental Facility (MLF) of Japan Proton Accelerator Research Complex (J-PARC). A $^3$He gas-filling station was constructed at J-PARC, and several $^3$He cells with long spin relaxation times have been fabricated using the gas-filling station. A laboratory has been prepared in the MLF beam hall for polarizing $^3$He cells, and compact pumping systems with laser powers of 30~W and 110~W, which can be installed onto a neutron beamline, have been developed. A $^3$He polarization of 85% was achieved at a neutron beamline by using the pumping system with the 110~W laser. Recently, the first user experiment utilizing the $^3$He spin filter was conducted, and there have been several more since then. The development and utilization of $^3$He spin filters at MLF of J-PARC are reported., Comment: 9 pages, 15 figures

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.

The evaluation of the magnetization distribution inside a bulk magnet is important for ensuring the performance of automotive motors because it strongly depends on the quality of magnetization inside the permanent magnet. In the conventional destructive method, it is difficult to accurately measure the magnetization with a high spatial resolution. The polarized neutron imaging technique can be used to visualize the distribution of the magnetic flux density inside a magnet nondestructively. In this study, we demonstrated the imaging of the magnetization distribution using polarized neutrons in an anisotropic ferrite magnet sample. The 2D distribution of the magnetization was experimentally obtained by polarized neutron imaging with a high spatial resolution of less than 1 mm. Furthermore, the validity of the results was confirmed by comparing them with those obtained using the conventional destructive method.