Comparing wire-mesh sensor with neutron radiography for measurement of liquid fraction in foam.

The liquid fraction of foam is an important quantity in engineering process control and essential to interpret foam rheology. Established measurement tools for the liquid fraction of foam, such as optical measurement or radiography techniques as well as weighing the foam, are mostly laboratory-based, whereas conductivity-based measurements are limited to the global measurement without detailed spatial information of liquid fraction. In this work, which combines both types of measurement techniques, the conductivity-based wire-mesh sensor is compared with neutron radiography. We found a linear dependency between the liquid fraction of the foam and the wire-mesh readings with a statistical deviation less than 15%. However, the wire-mesh sensor systematically overestimates the liquid fraction, which we attribute to liquid bridge formation between the wires.

Achromatic Non-Interferometric Single Grating Neutron Dark-Field Imaging.

We demonstrate a simple single grating beam modulation technique, which enables the use of a highly intense neutron beam for differential phase and dark-field contrast imaging and thus spatially resolved structural correlation measurements in full analogy to interferometric methods. In contrast to these interferometric approaches our method is intrinsically achromatic and provides unprecedented flexibility in the choice of experimental parameters. In particular the method enables straight forward application of quantitative dark-field contrast imaging in time-of-flight mode at pulsed neutron sources. Utilizing merely a macroscopic absorption mask unparalleled length scales become accessible. We present results of quantitative dark-field contrast imaging combining microstructural small angle scattering analyses with real space imaging for a variety of materials.

Visualizing the heterogeneous breakdown of a fractal microstructure during compaction by neutron dark-field imaging.

Structural properties of cohesive powders are dominated by their microstructural composition. Powders with a fractal microstructure show particularly interesting properties during compaction where a microstructural transition and a fractal breakdown happen before compaction and force transport. The study of this phenomenon has been challenging due to its long-range effect and the subsequent necessity to characterize these microstructural changes on a macroscopic scale. For the detailed investigation of the complex nature of powder compaction for various densification states along with the heterogeneous breakdown of the fractal microstructure we applied neutron dark-field imaging in combination with a variety of supporting techniques with various spatial resolutions, field-of-views and information depths. We used scanning electron microscopy to image the surface microstructure in a small field-of-view and X-ray tomography to image density variations in 3D with lower spatial resolution. Non-local spin-echo small-angle neutron scattering results are used to evaluate fitting models later used as input parameters for the neutron dark-field imaging data analysis. Finally, neutron dark-field imaging results in combination with supporting measurements using scanning electron microscopy, X-ray tomography and spin-echo small angle scattering allowed us to comprehensively study the heterogeneous transition from a fractal to a homogeneous microstructure of a cohesive powder in a quantitative manner.

Chasing quantitative biases in neutron imaging with scintillator-camera detectors: a practical method with black body grids.

We propose a method for improving the quantification of neutron imaging measurements with scintillator-camera based detectors by correcting for systematic biases introduced by scattered neutrons and other sources such as light reflections in the detector system. This method is fully experimental, using reference measurements with a grid of small black bodies (BB) to measure the bias contributions directly. Using two test samples, one made of lead alloy and having a moderate (20%) neutron transmission and one made of stainless-steel and having a very low (1%) transmission, we evaluated the improvement brought by this method in reducing both the average quantification bias and the uncertainty around this average bias after tomographic reconstruction. The results show that a reduction of the quantification bias of up to one order of magnitude can be obtained. For moderately transparent samples, little sensitivity is observed to the parameters used for the correction. For the more challenging sample with very low transmission, a correct placement of the BB grid is of utmost importance for a successful correction.

A Monte Carlo approach for scattering correction towards quantitative neutron imaging of polycrystals.

The development of neutron imaging from a qualitative inspection tool towards a quantitative technique in materials science has increased the requirements for accuracy significantly. Quantifying the thickness or the density of polycrystalline samples with high accuracy using neutron imaging has two main problems: (i) the scattering from the sample creates artefacts on the image and (ii) there is a lack of specific reference attenuation coefficients. This work presents experimental and simulation results to explain and approach these problems. Firstly, a series of neutron radiography and tomography experiments of iron, copper and vanadium are performed and serve as a reference. These materials were selected because they attenuate neutrons mainly through coherent (Fe and Cu) and incoherent (V) scattering. Secondly, an ad hoc Monte Carlo model was developed, based on beamline, sample and detector parameters, in order to simulate experiments, understand the physics involved and interpret the experimental data. The model, developed in the McStas framework, uses a priori information about the sample geometry and crystalline structure, as well as beamline settings, such as spectrum, geometry and detector type. The validity of the simulations is then verified with experimental results for the two problems that motivated this work: (i) the scattering distribution in transmission imaging and (ii) the calculated attenuation coefficients.

Unlocking high spatial resolution in neutron imaging through an add-on fibre optics taper.

The demand for high resolution neutron imaging has been steadily increasing over the past years. The number of facilities offering cutting edge resolution is however limited, due to (i) the design complexity of an optimized device able to reach a resolution in the order of ≈ 10 µm and (ii) limitations in available neutron flux. Here we propose a simple addition, based on a Fibre Optics Taper (FOT), that can be easily attached to an already existing scintillator-camera imaging detector in order to efficiently increase its spatial resolution and hence boost the capability of an instrument into high resolution applications.

Focussed ion beam nanotomography reveals the 3D morphology of different solid phases in hardened cement pastes.

Due to the development of integrated low-keV back-scattered electron detectors, it has become possible in focussed ion beam nanotomography to segment not only solid matter and porosity of hardened cement paste, but also to distinguish different phases within the solid matter. This paper illustrates a method that combines two different approaches for improving the contrast between different phases in the solid matrix of a cement paste. The first approach is based on the application of a specially developed 3D diffusion filter. The second approach is based on a modified data-acquisition procedure during focussed ion beam nanotomography. A pair of electron images is acquired for each slice in the focussed ion beam nanotomography dataset. The first image is captured immediately after ion beam milling; the second image is taken after a prolonged exposure to electron beam scanning. The acquisition of complementary focussed ion beam nanotomography datasets and processing the images with a 3D anisotropic diffusion filter allows distinguishing different phases within the hydration products.

Limitation in obtainable surface roughness of hardened cement paste: 'virtual' topographic experiment based on focussed ion beam nanotomography datasets.

Surface roughness affects the results of nanomechanical tests. The surface roughness values to be measured on a surface of a porous material are dependent on the properties of the naturally occurring pore space. In order to assess the surface roughness of hardened cement paste (HCP) without the actual influence of the usual sample preparation for nanomechanical testing (i.e. grinding and polishing), focussed ion beam nanotomography datasets were utilized for reconstruction of 3D (nanoscale resolution) surface profiles of hardened cement pastes. 'Virtual topographic experiments' were performed and root mean square surface roughness was then calculated for a large number of such 3D surface profiles. The resulting root mean square (between 115 and 494 nm) is considerably higher than some roughness values (as low as 10 nm) reported in the literature. We suggest that thus-analysed root mean square values provide an estimate of a 'hard' lower limit that can be achieved by 'artefact-free' sample preparation of realistic samples of hardened cement paste. To the best of our knowledge, this 'hard' lower limit was quantified for a porous material based on hydraulic cement for the first time. We suggest that the values of RMS below such a limit may indicate sample preparation artefacts. Consequently, for reliable nanomechanical testing of disordered porous materials, such as hardened cement paste, the preparation methods may require further improvement.

3D imaging of microstructure of spruce wood.

Synchrotron radiation phase-contrast X-ray tomographic microscopy (srPCXTM) was applied to observation and identification of the features of spruce anatomy at the cellular lengthscale. The pilot experiments presented in the paper clearly revealed the features of the heartwood of Spruce (Picea abies [L.] Karst.), such as lumina and pits connecting the lumina, with a theoretical voxel size of 0.7 x 0.7 x 0.7 microm(3). The experiments were carried out on microspecimens of heartwood, measuring approximately 200 by 200 micrometers in cross-section. The technique for production and preparation of wood microsamples was developed within the framework of this investigation. The total porosity of the samples was derived and the values of the microstructural parameters, such as the diameters of tracheid, cell wall thicknesses and pit diameters were assessed non-invasively. Microstructural features as thin/small as approximately 1.5 microm were revealed and reconstructed in 3D. It is suggested that the position of sub-voxel-sized features (such as position of tori in the bordered pit pairs) can be determined indirectly using watershed segmentation. Moreover, the paper discusses the practical issues connected with a pipelined phase-contrast synchrotron-based microtomography experiment and the possible future potentials of this technique in the domain of wood science.