Saurabh Kabra

Materials analysis opportunities on the new neutron imaging facility IMAT@ISIS

A new neutron imaging and diffraction facility, called IMAT, is currently being commissioned at the ISIS pulsed neutron spallation source. IMAT will take advantage of neutron time-of-flight measurement techniques for flexible neutron energy selection and effective energy discrimination. The instrument will be completed and commissioned within the next few months, after neutrons have been recently delivered to the sample area. From 2016 IMAT will enable white-beam neutron radiography and tomography as well as energy-dependent neutron imaging. The facility will offer a spatial resolution down to 50 microns for a field of view of up to 400 cm2. IMAT will be operated as a user facility for material science applications and will be open for developments of time-of-flight imaging methods.

Phase transition and ordering behavior of ternary Ti–Al–Mo alloys using in-situ neutron diffraction

Abstract Neutron diffraction has been used for in-situ investigations to elucidate the phase transformation behavior of two Mo-containing TiAl alloys with compositions of Ti-44Al-3Mo and Ti-44Al-7Mo (in at.%). Five different phases are present in these alloys. These include three ordered phases at room temperature, namely α2, β0 and γ and two disordered phases, and, which occur at higher temperatures. The sequence of the three phase transformations in each alloy has been determined. The phase transformation and disordering/ordering temperatures were determined on heating and cooling from the diffracted peak intensities. The neutron experiments are particularly sensitive to the order–disorder transitions in TiAl alloys, which are compared with the overall phase fractions obtained from previous high energy X-ray diffraction. Hysteresis and undercooling effects are observed for the various phase transformations and depend on the nature of atomic rearrangements.

Texture analysis with a time‐of‐flight neutron strain scanner

A time-of-flight (TOF) neutron strain scanner is a white-beam instrument optimized to measure diffractograms at precise locations within bulky specimens, typically along two perpendicular sample orientations. Here, a method is proposed that exploits the spatial resolution (∼1 mm) provided by such an instrument to determine in a nondestructive manner the crystallographic texture at selected locations within a macroscopic object. The method is based on defining the orientation distribution function (ODF) of the crystallites from several incomplete pole figures, and it has been implemented on ENGIN-X, a neutron strain scanner at the ISIS facility in the UK. This method has been applied to determine the texture at different locations of Al alloy plates welded along the rolling direction and to study a Zr2.5%Nb pressure tube produced for a CANDU nuclear power plant. For benchmarking, the results obtained with this instrument for samples of ferritic steel, copper, Al alloys and Zr alloys have been compared with measurements performed using conventional X-ray diffractometers and more established neutron techniques. For cases where pole figure coverage is incomplete, the use of TOF neutron transmission measurements simultaneously performed on the specimens is proposed as a simple and powerful test to validate the resulting ODF.

Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

Defect dynamics in polycrystalline zirconium alloy probed in situ by primary extinction of neutron diffraction

After α + β-zirconium has fully transformed into β-phase upon heating, the intensities of all β-Zr Bragg reflections decrease simultaneously as a function of time. It is shown that this effect represents a transition from the kinematic to the dynamic theory of diffraction due to the ever increasing crystal perfection driven by thermal recovery of the system. The best fitting coherent crystallite size of 30 μm and other microstructural features are verified by in situ laser scanning confocal microscopy. This effect of primary extinction in neutron diffraction has been employed to further investigate the crystal perfection kinetics. Upon further heating, crystal recovery is identified as a process of dislocation annihilation, suffering from lattice friction. Upon cooling, precipitating α-Zr induces strain into the perfect β-crystallites, re-establishing the kinematic diffraction intensities. An Avrami analysis leads to the estimations of nucleation time, consumption of nucleation sites and lower-dimensional growth. Such technique bears great value for further investigation on all metal systems annealed close to the melting temperature.

Flexible sample environment for high resolution neutron imaging at high temperatures in controlled atmosphere

High material penetration by neutrons allows for experiments using sophisticated sample environments providing complex conditions. Thus, neutron imaging holds potential for performing in situ nondestructive measurements on large samples or even full technological systems, which are not possible with any other technique. This paper presents a new sample environment for in situ high resolution neutron imaging experiments at temperatures from room temperature up to 1100 °C and/or using controllable flow of reactive atmospheres. The design also offers the possibility to directly combine imaging with diffraction measurements. Design, special features, and specification of the furnace are described. In addition, examples of experiments successfully performed at various neutron facilities with the furnace, as well as examples of possible applications are presented. This covers a broad field of research from fundamental to technological investigations of various types of materials and components.

Sample environment for neutron scattering measurements of internal stresses in engineering materials in the temperature range of 6 K to 300 K

Internal stresses in materials have a considerable effect on material properties including strength, fracture toughness, and fatigue resistance. The ENGIN-X beamline is an engineering science facility at ISIS optimized for the measurement of strain and stress using the atomic lattice planes as a strain gauge. Nowadays, the rapidly rising interest in the mechanical properties of engineering materials at low temperatures has been stimulated by the dynamic development of the cryogenic industry and the advanced applications of the superconductor technology. Here we present the design and discuss the test results of a new cryogenic sample environment system for neutron scattering measurements of internal stresses in engineering materials under a load of up to 100 kN and in the temperature range of 6 K to 300 K. Complete cooling of the system starting from the room temperature down to the base temperature takes around 90 min. Understanding of internal stresses in engineering materials at cryogenic temperatures is vital for the modelling and designing of cutting-edge superconducting magnets and other superconductor based applications.

Compressive behaviour of nanocrystalline Mg–5Al alloys

Abstract Magnesium alloys are attracting increasing research interests due to their low density, high specific strength, good machinability and availability as compared to other structural materials. However, the deformation and failure mechanisms of nanocrystalline (nc) Mg alloys have not been well understood. In this work, the deformation behaviour of nc Mg–5Al alloys was investigated using compression test, with focus on the effects of grain size. The average grain size of the Mg–Al alloy was changed from 13 to 50 nm via mechanical milling. The results showed that grain size had a significant influence on the yield stress and ductility of the Mg alloys, and the materials exhibited increased strain rate sensitivity with a decrease in grain size. The deformation mechanisms were also strongly dependent on the grain sizes.

Measurement and Simulation of Residual Strain in a Laser Welded Titanium Ring

Elastic residual strains were measured in a laser welded commercially pure titanium ring using a non-destructive neutron diffraction technique in order to determine the resolution of this method for the characterization of small laser welds. In addition, these measurements were used to validate calculations made using residual strain data obtained from simulation of the residual stress near the weld. The measured strains were in good agreement with the simulated results.

Phase composition mapping of a 17th century Japanese helmet

Neutron Diffraction represents the ideal technique for the characterisation of the micro-structural properties of ancient metals, allowing retrieval of information on the smelting process, and the mechanical and thermal treatments applied during the manufacture of the sample. The object under investigation is a 17th century Japanese helmet (kabuto) from the Haruta School that has already been analysed, along with other six similar examples, using a general purpose neutron diffractometer. Through this study, the quality of the steel (phase composition) was determined and information on the thermo-mechanical treatments applied was inferred, averaging over a scattering volume that affected the entire thickness of the sample. The Haruta kabuto stood out for its very high carbon content, the absence of texture and residual strain, and very big grain size. These factors and the presence of incomplete reduction of the ore sand suggest the presence of plates with a composite structure of layers of steel and iron superimposed. This paper shows the possibility of using neutron diffraction on a highly collimated instrument, such as ENGIN-X (ISIS, UK), to be able to select a very small gauge volume and, this way, to detect variations in the phase composition along the thickness of the plates. Here we present novel results from diffraction measurements by using the instrument ENGIN-X. This study completes the previous cycle of neutron measurements on this sample and sheds light on the structure of the plates.