Bjorn Clausen

Non-destructive evaluation of plastically deformed metals, particularly diffraction line profile analysis (DLPA), is valuable both to estimate dislocation densities and arrangements and to validate microstructure-aware constitutive models. To date, the interpretation of whole line diffraction profiles relies on the use of semi-analytical models such as the extended convolutional multiple whole profile (eCMWP) method. This study introduces and validates two data-driven DLPA models to extract dislocation densities from experimentally gathered whole line diffraction profiles. Using two distinct virtual diffraction models accounting for both strain and instrument induced broadening, a database of virtual diffraction whole line profiles of Ta single crystals is generated using discrete dislocation dynamics. The databases are mined to create Gaussian process regression-based surrogate models, allowing dislocation densities to be extracted from experimental profiles. The method is validated against 11 experimentally gathered whole line diffraction profiles from plastically deformed Ta polycrystals. The newly proposed model predicts dislocation densities consistent with estimates from eCMWP. Advantageously, this data driven LPA model can distinguish broadening originating from the instrument and from the dislocation content even at low dislocation densities. Finally, the data-driven model is used to explore the effect of heterogeneous dislocation densities in microstructures containing grains, which may lead to more accurate data-driven predictions of dislocation density in plastically deformed polycrystals.

Polycrystalline materials can have complex anisotropic properties depending on their crystallographic texture and crystal structure. In this study, we use resonant ultrasound spectroscopy (RUS) to nondestructively quantify the elastic anisotropy in extruded aluminum alloy 1100-O, an inherently low-anisotropy material. Further, we show that RUS can be used to indirectly provide a description of the material’s texture, which in the present case is found to be transversely isotropic. By determining the entire elastic tensor, we can identify the level and orientation of the anisotropy originated during extrusion. The relative anisotropy of the compressive (c₁₁/c₃₃) and shear (c₄₄/c₆₆) elastic constants is 1.5% ± 0.5% and 5.7% ± 0.5%, respectively, where the elastic constants (five independent elastic constants for transversely isotropic) are those associated with the extrusion axis that defines the symmetry of the texture. These results indicate that the texture is expected to have transversely isotropic symmetry. This finding is confirmed by two additional approaches. First, we confirm elastic constants and the degree of elastic anisotropy by direct sound velocity measurements using ultrasonic pulse echo. Second, neutron diffraction (ND) data confirm the symmetry of the bulk texture consistent with extrusion-induced anisotropy, and polycrystal elasticity simulations using the elastic self-consistent model with input from ND textures and aluminum single-crystal elastic constants render similar levels of polycrystal elastic anisotropy to those measured by RUS. We demonstrate the ability of RUS to detect texture-induced anisotropy in inherently low-anisotropy materials. Therefore, as many other common materials have intrinsically higher elastic anisotropy, this technique should be applicable for similar levels of texture, providing an efficient general diagnostic and characterization tool.

A simple statistical analysis which yields the precision, resolution, accuracy and trueness of diffraction-based lattice strain measurements is discussed. The procedure consists of measuring the thermal expansion induced in each component of an ideal non-reacting two-component crystalline powder sample in situ. One component, with a high coefficient of thermal expansion (CTE), serves as an internal thermometer. The quantities of interest are obtained by determining the smallest statistically significant thermal lattice strain which can be detected through diffraction analysis in the second, low-CTE, component in response to controlled temperature changes. This procedure also provides a robust check of the alignment of the diffraction system and is able to reveal the presence of systematic errors. The application of this technique to a time-of-flight engineering diffractometer/strain scanner is presented.

The effects of athermal martensite on yielding behavior and strain partitioning during deformation is explored using in situ neutron diffraction for a 0.14C–7.14Mn medium manganese steel. Utilizing a novel heat treatment, termed double soaking, samples with similar microstructural composition and varied athermal martensite strength and microstructural characteristics, which composed the bulk of the matrix phase, were characterized. It was found that the addition of either as-quenched or tempered athermal martensite led to an improvement in mechanical properties as compared to a ferrite plus austenite medium manganese steel, although the yielding and work hardening behavior were highly dependent upon the martensite characteristics. Specifically, athermal martensite was found to promote continuous yielding and improve the work hardening rate during deformation. The results of this study are particularly relevant when considering the effect of post-processing thermal heat treatments, such as tempering or elevated temperature service environments, on the mechanical properties of medium manganese steels containing athermal martensite.

Pervasive deformation twinning in magnesium greatly affects its strength and formability. The local stress fields associated with twinning play a key role on deformation behavior and fracture but are extremely difficult to characterize experimentally. In this study, we perform synchrotron experiments with differential-aperture X-ray microscopy to measure the 3D stress fields in the vicinity of a twin with a spatial resolution of 0.5 micrometer. The measured local stress field aids to identify the sequence of events involved with twinning. We find that the selected grain deforms elastically before twinning, and the twin formation splits the grain into two non-interacting domains. Under further straining one domain of the grain continued to deform elastically, whereas the other domain deforms plastically by prismatic slip. This heterogeneous deformation behavior may be mediated by the surrounding medium and it is likely to lead to asymmetric twin growth.

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residual strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. Knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.

In-situ time-of-flight neutron diffraction experiments were conducted on the uranium-niobium alloy with 6 wt. % Nb (U–6Nb) at pressures up to 4.7 GPa and temperatures up to 1073 K. Upon static compression at room temperature, the monoclinic structure of U–6Nb (α″ U–6Nb) remains stable up to the highest experimental pressure. Based on the pressure-volume measurements at room temperature, the least-squares fit using the finite-strain equation of state (EOS) yields an isothermal bulk modulus of B0 = 127 ± 2 GPa for the α″-phase of U–6Nb. The calculated zero-pressure bulk sound speed from this EOS is 2.706 ± 0.022 km/s, which is in good agreement with the linear extrapolation of the previous Hugoniot data above 12 GPa for α″ U–6Nb, indicating that the dynamic response under those shock-loading conditions is consistent with the stabilization of the initial monoclinic phase of U-6Nb. Upon heating at ambient and high pressures, the metastable α″ U–6Nb exhibits complex transformation paths leading to the diffusional phase decomposition, which are sensitive to applied pressure, stress state, and temperature-time path. These findings provide new insight into the behavior of atypical systems such as U-Nb and suggest that the different U-Nb phases are separated by rather small energies and hence highly sensitive to compositional, thermal, and mechanical perturbations.

In-situ time-of-flight neutron diffraction experiments were conducted on the uranium-niobium alloy with 6 wt. % Nb (U–6Nb) at pressures up to 4.7 GPa and temperatures up to 1073 K. Upon static compression at room temperature, the monoclinic structure of U–6Nb (α″ U–6Nb) remains stable up to the highest experimental pressure. Based on the pressure-volume measurements at room temperature, the least-squares fit using the finite-strain equation of state (EOS) yields an isothermal bulk modulus of B0 = 127 ± 2 GPa for the α″-phase of U–6Nb. The calculated zero-pressure bulk sound speed from this EOS is 2.706 ± 0.022 km/s, which is in good agreement with the linear extrapolation of the previous Hugoniot data above 12 GPa for α″ U–6Nb, indicating that the dynamic response under those shock-loading conditions is consistent with the stabilization of the initial monoclinic phase of U-6Nb. Upon heating at ambient and high pressures, the metastable α″ U–6Nb exhibits complex transformation paths leading to the diffusional phase decomposition, which are sensitive to applied pressure, stress state, and temperature-time path. These findings provide new insight into the behavior of atypical systems such as U-Nb and suggest that the different U-Nb phases are separated by rather small energies and hence highly sensitive to compositional, thermal, and mechanical perturbations.

Triaminotrinitrobenzene (TATB) is a highly anisotropic molecular crystal used in several plastic-bonded explosive (PBX) formulations. A complete understanding of the orientation distribution of TATB particles throughout a PBX charge is required to understand spatially variable, anisotropic macroscale properties of the charge. Although texture of these materials can be measured after they have been subjected to mechanical or thermal loads, measuring texture evolution in situ is important in order to identify mechanisms of crystal deformation and reorientation used to better inform thermomechanical models. Neutron diffraction measurements were used to estimate crystallographic reorientation while deuterated TATB (d-TATB) powder was consolidated into a cylindrical pellet via a uniaxial die-pressing operation at room temperature. Both the final texture of the pressed pellet and the in situ evolution of texture during pressing were measured, showing that the d-TATB grains reorient such that (001) poles become preferentially aligned with the pressing direction. A compaction model is used to predict the evolution of texture in the pellet during the pressing process, finding that the original model overpredicted the texture strength compared to these measurements. The theory was extended to account for initial particle shape and pore space, bringing the results into good agreement with the data.

The ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni₂TiAl/NiAl or single-Ni₂TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior between the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate.

The evolution of deformation mechanisms in randomly textured magnesium alloy during uniaxial and biaxial mechanical tests has been monitored using concurrent application of acoustic emission and neutron diffraction methods. The influence of the loading path on both twinning and dislocation slip is discussed in detail. It is shown that both the twinning and non-basal slip are sensitive to the loading direction.

An understanding of load sharing among constituent phases aids in designing mechanical properties of multiphase materials. Here we investigate load partitioning between the body-centered-cubic iron matrix and NiAl-type precipitates in a ferritic alloy during uniaxial tensile tests at 364 and 506 °C on multiple length scales by in situ neutron diffraction and crystal plasticity finite element modeling. Our findings show that the macroscopic load-transfer efficiency is not as high as that predicted by the Eshelby model; moreover, it depends on the matrix strain-hardening behavior. We explain the grain-level anisotropic load-partitioning behavior by considering the plastic anisotropy of the matrix and elastic anisotropy of precipitates. We further demonstrate that the partitioned load on NiAl-type precipitates relaxes at 506 °C, most likely through thermally-activated dislocation rearrangement on the microscopic scale. The study contributes to further understanding of load-partitioning characteristics in multiphase materials.

Triaminotrinitrobenzene (TATB) is a highly anisotropic molecular crystal used in several plastic‐bonded explosive (PBX) formulations. TATB‐based explosives exhibit irreversible volume expansion (“ratchet growth”) when thermally cycled. A theoretical understanding of the relationship between anisotropy of the crystal, crystal orientation distribution (texture) of polycrystalline aggregates, and the intergranular interactions leading to this irreversible growth is necessary to accurately develop physics‐based predictive models for TATB‐based PBXs under various thermal environments. In this work, TATB lattice parameters were measured using neutron diffraction during thermal cycling of loose powder and a pressed pellet. The measured lattice parameters help clarify conflicting reports in the literature as these new results are more consistent with one set of previous results than another. The lattice parameters of pressed TATB were also measured as a function of temperature, showing some differences from the powder. This data is used along with anisotropic single‐crystal stiffness moduli reported in the literature to model the nominal stresses associated with intergranular constraints during thermal expansion. The texture of both specimens were characterized and the pressed pellet exhibits preferential orientation of (001) poles along the pressing direction, whereas no preferred orientation was found for the loose powder. Finally, thermal strains for single‐crystal TATB computed from lattice parameter data for the powder is input to a self‐consistent micromechanical model, which predicts the lattice parameters of the constrained TATB crystals within the pellet. The agreement of these model results with the diffraction data obtained from the pellet is discussed along with future directions of research.

In-situ neutron diffraction during cyclic tension-compression loading (∼+3.5% to −2.8%) of a 17Mn-3Al-2Si-1Ni-0.06C steel that exhibits concurrent transformation and twinning -induced plasticity effects indicated a significant contribution of intragranular back stresses to the observed Bauschinger effect. Rietveld analysis revealed a higher rate of martensitic transformation during tension compared to compression. Throughout cycling, α′-martensite exhibited the highest phase strains such that it bears an increasing portion of the macroscopic load as its weight fraction evolves. On the other hand, the ε-martensite strain remained compressive as it accommodated most of the internal strains caused by the shape misfit associated with the γ→ε and/or ε→α′ transformations.

A novel diffraction-based method has been developed to determine the substructure in terms of the fraction of prevailing slip systems and dislocation densities in multiple individual texture components of strongly textured materials. The method was applied to a strongly textured cold-rolled Zircaloy-2 sample, compressed along the normal direction of the rolled plate. Fourteen diffraction patterns were collected by time-of-flight neutron diffraction experiments at seven different purposely selected sample orientations. The diffraction peaks corresponding only to one single texture component out of the four prevailing components were identified and used to construct texture-specific diffraction patterns. The best five such patterns were evaluated by the convolutional multiple whole profile procedure of line profile analysis for the fractions of the prevailing 〈a〉-, 〈c + a〉- and 〈c〉-type slip systems and the corresponding dislocation densities. It is found that in the three texture components with thecaxis not parallel to the normal direction of rolling the average dislocation densities and fractions of slip-system types are the same. However, in the texture component with thecaxis parallel to the normal direction of rolling the fraction of the 〈a〉-type slip system is somewhat smaller than in the other components and that of the 〈c〉-type slip system is somewhat larger than zero. The fractions of the prevailing slip systems are in good correlation with literature data of self-consistent polycrystal plasticity modeling of Zircaloy-2.

There have been numerous efforts to develop creep-resistant materials strengthened by incoherent particles at high temperatures and stresses in response to future energy needs for steam turbines in thermal-power plants. However, the microstructural instability of the incoherent-particle-strengthened ferritic steels limits their application to temperatures below 900 K. Here, we report a novel ferritic alloy with the excellent creep resistance enhanced by coherent hierarchical precipitates, using the integrated experimental (transmission-electron microscopy/scanning-transmission-electron microscopy,in-situneutron diffraction and atom-probe tomography) and theoretical (crystal-plasticity finite-element modeling) approaches. This alloy is strengthened by nano-scaled L2₁-Ni₂TiAl (Heusler phase)-based precipitates, which themselves contain coherent nano-scaled B2 zones. These coherent hierarchical precipitates are uniformly distributed within the Fe matrix. Our hierarchical structure material exhibits the superior creep resistance at 973 K in terms of the minimal creep rate, which is four orders of magnitude lower than that of conventional ferritic steels. These results provide a new alloy-design strategy using the novel concept of hierarchical precipitates and the fundamental science for developing creep-resistant ferritic alloys. The present research will broaden the applications of ferritic alloys to higher temperatures.

NeXus is an effort by an international group of scientists to define a common data exchange and archival format for neutron, X-ray and muon experiments. NeXus is built on top of the scientific data format HDF5 and adds domain-specific rules for organizing data within HDF5 files, in addition to a dictionary of well defined domain-specific field names. The NeXus data format has two purposes. First, it defines a format that can serve as a container for all relevant data associated with a beamline. This is a very important use case. Second, it defines standards in the form of application definitions for the exchange of data between applications. NeXus provides structures for raw experimental data as well as for processed data.

The aim of this work is to understand the evolutions of the β₁metastable austenite phase of a CuAlBe Shape Memory Alloy at macroscopic and microscopic scales under mechanical solicitation by neutron diffraction. The tensile specimen, taken in the raw material is subjected to superelastic cycles at room temperature on SMARTS diffractometer. Before loading, the mater ial is fully austenitic. During loading, after elastic deformation of austenite, phase transformation starts, martensite variants appear. The material follows a law of pseudo elastic behavior. At the end of the first mechanical cycle after unloading, the macroscopic curve does not fully return into its original point. A macroscopic deformation is observed. The evolution of first order microdeformations during mechanical cycles shows a large deformation of {400} plane family. This deformation is linked to the presence of <001> partial fibber characterizing the crystallographic texture of the material after elaboration. The FWHM of the (400) diffraction peak is also largely increased during loading. This increase is the signature of the generation of stacking faults during the transformation of β₁metastable austenite into β₁martensite.

Time-of-flight neutron measurements have been made at 20, 400 and 650oC on δ-processed Inconel 718 in order to measure the load sharing between the γ-phase matrix and the orthorhombic δ-phase. The strain response parallel and perpendicular to the applied stress was measured for seven γ-phase reflections and five δ-phase reflections. The latter were about 50 times weaker than the former suggesting a 2.0% concentration of the δ-phase. At all temperatures the δ-phase strain becomes strongly tensile parallel to the loading direction but also exhibits plastic deformation. However, the nature of the three orthorhombic strains changes with temperature.

Time-of-flight neutron measurements have been made at 20, 400 and 650oC on δ-processed Inconel 718 in order to measure the load sharing between the γ-phase matrix and the orthorhombic δ-phase. The strain response parallel and perpendicular to the applied stress was measured for seven γ-phase reflections and five δ-phase reflections. The latter were about 50 times weaker than the former suggesting a 2.0% concentration of the δ-phase. At all temperatures the δ-phase strain becomes strongly tensile parallel to the loading direction but also exhibits plastic deformation. However, the nature of the three orthorhombic strains changes with temperature.

The high-resolution neutron diffraction and acoustic emission (AE) techniques have been used for in-situ investigation of deformation twinning and microstructure evolution in cast polycrystalline magnesium. The combination of these two techniques results in obtaining complementary information about the twinning mechanism and evolution of the dislocation structure during the straining. The dependence of the mechanisms of the plastic deformation on loading mode is discussed in detail. The microscopy investigations revealed a difference in twin number and size after tension and compression, respectively.

Simultaneous use of neutron diffraction and attenuation based transmission Bragg edge imaging for strain measurements is demonstrated in this paper using the pulse neutron source at Los Alamos National Laboratory. Cylindrical samples made from ferritic steel have been subjected to in-situ elastic loading in tension and torsion. Lattice strains were investigated for both deformation modes by time-of-flight (TOF) neutron diffraction using two detector banks at 2θ of ±90°. At the same time, the transmitted portion of the neutron beam was recorded with the goal to analyze the position and shape of the Bragg edges, using a novel time/energy resolved Microchannel Plate (MCP) detector with pixel size of 55 µm and a 28x28 mm² field of view. Lattice strains obtained using neutron diffraction indicate that the deformation path (tension versus torsion) has important effect on their evolution and related results are summarized.

The emphasis of this paper is to explain the aspects of the experimental setup and data interpretation associated with neutron Bragg edge transmission technique for obtaining through-thickness averaged strain measurements. Implications of using transmission imaging based strain mapping for samples subjected to deformation under tensile loading (where stress at a given cross-section is constant) versus torsional loading (where stress varies linearly from center to outer radius) are discussed. In the case of samples subjected to tensile loading, analysis of the Bragg edge shifts provides the strain value in the direction of the transmitted beam. Thus, three strain components are measured simultaneously when performing Bragg edge imaging in addition to diffraction using two detector banks. For specimens subjected to pure shear by torsion, the Bragg edge transmission technique cannot readily provide quantitative strain information as the mid-point of the Bragg edge does not shift uniformly due to external loading, but results in a broadening of the Bragg edge. Such information can be used to describe the variation of strain distribution along the transmitted beam direction. Spatially resolved Bragg edge maps will be very helpful to detect d-spacing inhomogeneities within the illuminated volume, which may remain undetected when using diffraction only measurements.

Time-of-flight neutron diffraction, contour method, and surface hole drilling residual stress measurements were conducted at Los Alamos National Lab (LANL) on a lab sized plate specimen (P4) from phase 1 of the joint U.S. Nuclear Regulatory Commission and Electric Power Research Institute Weld Residual Stress (NRC/EPRI WRS) program. The specimen was fabricated from a 304L stainless steel plate containing a seven pass alloy 82 groove weld, restrained during welding and removed from the restraint for residual stress characterization. This paper presents neutron diffraction and contour method results, and compares these experimental stress measurements to a WRS finite element (FE) model. Finally, details are provided on the procedure used to calculate the residual stress distribution in the restrained or as welded condition in order to allow comparison to other residual stress data collected as part of phase 1 of the WRS program.

A novel capability was designed, implemented, and tested for in situ neutron diffraction measurements during loading at cryogenic temperatures on the spectrometer for materials research at temperature and stress at Los Alamos National Laboratory. This capability allowed for the application of dynamic compressive forces of up to 250 kN on standard samples controlled at temperatures between 300 and 90 K. The approach comprised of cooling thermally isolated compression platens that in turn conductively cooled the sample in an aluminum vacuum chamber which was nominally transparent to the incident and diffracted neutrons. The cooling/heat rate and final temperature were controlled by regulating the flow of liquid nitrogen in channels inside the platens that were connected through bellows to the mechanical actuator of the load frame and by heaters placed on the platens. Various performance parameters of this system are reported here. The system was used to investigate deformation in Ni–Ti–Fe shape memory alloys at cryogenic temperatures and preliminary results are presented.

Neutron diffraction measurements of strain in austenitic stainless steel alloys are presented to examine whether there are contributions to the shifts from deformation induced stacking faults. Differences between successive orders of reflections are consistent with the presence of stacking faults for 316 stainless steel but not for a NiCrFe steel.

In this study, the mechanical behavior of porous thermally microcracked ceramics has been compared with that of solely porous materials, under compressive applied stress. The different aspects of the micro and macroscopic stress-strain curves have been inserted into a coherent analytical model and compared with finite element modeling calculations. The agreement between experiments and models is very good. It is shown that mechanical microcracking, as opposed to thermal, introduces an irreversible aspect in the deformation mechanisms of porous ceramics. In this concern, mechanical loads differentiate themselves from thermal cycling. This leads for instance to a change of the Young’s modulus as a function of applied load, which qualifies those materials as visco-elastic.

In order to test new theories for residual stress measurement or to test the effects of residual stress on fatigue, fracture, and stress corrosion cracking, a known stress test specimen was designed and then fabricated, modeled, and experimentally validated. To provide a unique biaxial stress state, a 60 mm diameter 10 mm thick disk of 316L stainless steel was plastically compressed through the thickness with an opposing 15 mm diameter hard steel indenters in the center of the disk. For validation, the stresses in the specimen were first mapped using time-of-flight neutron diffraction and Rietveld full pattern analysis. Next, the hoop stresses were mapped on a cross section of two disks using the contour method. The contour results were very repeatable and agreed well with the neutron results. The indentation process was modeled using the finite element method. Because of a significant Bauschinger effect, accurate modeling required testing the cyclic behavior of the steel and then modeling it using a Chaboche-type combined hardening law. The model results agreed very well with the measurements. The duplicate contour measurements demonstrated stress repeatability better than 0.01% of the elastic modulus and allowed discussion of implications of measurements of parts with complicated geometries.

We report on in situ neutron diffraction measurements during heating and cooling through the phase transformation in shape memory NiTi. The lattice plane specific strain evolution remains linear with temperature and is not influenced by intergranular stresses, enabling the determination of the thermal expansion tensor of B19′ NiTi. The neutron measurements are consistent with macroscopic dilatometric measurements and a 30 000 grain polycrystalline self-consistent model. The accommodative nature of B19′ NiTi results in macroscopic shape changes being offset (with temperature) from the start and finish of the transformation. The texture does not evolve in the absence of biasing stresses.

Although ceramics are considered linear elastic materials, we have observed a non‐linear pseudo‐elastic behavior in porous cellular microcracked ceramics such as β‐eucryptite. This is attributed to the evolution of microstructure in these materials. This behavior is particularly different from that of non‐microcracked ceramics such as silicon carbide. It is shown that in microcracked materials two processes, namely stiffening and softening, always compete when a compressive external load is applied. The first regime is attributed to microcrack closure, and the second to microcracks opening, i.e. to a damage introduced by the applied stress. On the other hand rather a continuous damage is observed in the non‐microcracked case. A comparison has been done between the microscopic (as measured by neutron diffraction) and the macroscopic stress‐strain response. Also, it has been found that at constant load a significant strain relaxation occurs, which has two timescales, possibly driven by the two phenomena quoted above. Indeed, no such relaxation is observed for non‐microcracked SiC. Implications of these findings are discussed.

Residual strain profiles in friction-stir processed (FSP) AZ31B magnesium-alloy plates were measured using neutron diffraction. Two different specimens were prepared to investigate the influences of the tool shoulder and the tool pin on the residual-strain profiles: (Case 1) a plate processed with both the stirring pin and tool shoulder, i.e., a regular FSP plate subjected to both the plastic deformation and frictional heating, and (Case 2) a plate processed only with the tool shoulder, i.e., subjected mainly to the frictional heating. The results show that the strain profiles of both cases are qualitatively quite similar. The longitudinal strain is mainly tensile with its maximum near the bead of the FSP plate. On the other hand, the transverse and normal strains are mildly compressive in both Cases 1 and 2.

A comparison has been made between weld stresses in a Zircaloy-4 weld obtained by fitting individual peaks of the diffraction spectrum and by fitting the complete pattern by the Rietveld method. For the as-welded case there was satisfactory agreement between the two approaches. For the as-annealed case the agreement is less satisfactory possibly because of systematic errors in the “stress-free references”. It is suggested that the reference samples should have been cut from an annealed companion weld rather than by annealing the reference samples originally cut from the as-welded sample.

The evolution of temperature and thermal stresses during friction stir welding of Al6061-T6 was investigated by means of in situ, time resolved neutron diffraction technique. A method was developed to deconvolute the temperature and stress from the lattice spacing changes measured by neutron diffraction. The deep penetration capability of neutrons made it possible for the first time to obtain the temperature and thermal stresses inside a friction stir weld.

An ultrafine-grained steel with an average grain size of about 350nm was developed. The tensile testing at ambient temperature shows a threefold increase in the yield strength compared to its coarse-grained counterpart. Moreover, the increase in the strength was achieved without the sacrifice of the ductility due to strain-induced martensitic transformation. The evolution of lattice strains and phase fractions of the austenite and martensite phases during the deformation was investigated using in situ neutron diffraction to provide a micromechanical understanding of the transformation-induced plasticity responsible for the combination of high strength and ductility.

In situ neutron diffraction measurements during loading have been performed on plastically deformed superelastic NiTi samples. The measurements observed retained B19′ phase in the unloaded state as a result of the plastic deformation in otherwise completely B2 phase samples. A reversible stress-induced B2–B19′ transformation on application and removal of stress occurred in the presence of this retained B19′ phase. The amount and orientation of this retained B19′ phase changed with cycling. Such direct atomic scale observations in the bulk are used here for the first time to qualitatively elucidate the macroscopic stress-strain response in plastically deformed superelastic NiTi.

The atomic pair distribution function (PDF) approach has been used to study the local structure of liquids, glasses and disordered crystalline materials. In this paper, we demonstrate the use of the PDF method to investigate systems containing a crystalline and an amorphous structural phase. We present two examples: Bulk metallic glass with crystalline reinforcements and Fontainebleau sandstone, where an unexpected glassy phase was discovered. In this paper we also discuss the refinement methods used in detail.

Repeatable, hysteretic loops in quasi‐static loading measurements on rocks are well known; the fundamental processes responsible for them are not. The grain contact region is usually treated as the site of these processes, but there is little supporting experimental evidence. We have performed simultaneous neutron diffraction and quasi‐static loading experiments on a selection of rocks to experimentally isolate the response of these contact regions. Neutron diffraction measures strain in the lattice planes of the bulk of the grain material, so differences between this strain and the macroscopic response yield information about grain contact behavior. We find the lattice responds linearly to stress in all cases, oblivious to the macroscopic unrecoverable strains, curvature, and hysteresis, localizing these effects to the contacts. Neutron diffraction shows that the more granular rocks appear to distribute stresses so that the same strain appears in all the grains, independent of crystallographic orientation.

Repeatable, hysteretic loops in quasi‐static loading measurements on rocks are well known; the fundamental processes responsible for them are not. The grain contact region is usually treated as the site of these processes, but there is little supporting experimental evidence. We have performed simultaneous neutron diffraction and quasi‐static loading experiments on a selection of rocks to experimentally isolate the response of these contact regions. Neutron diffraction measures strain in the lattice planes of the bulk of the grain material, so differences between this strain and the macroscopic response yield information about grain contact behavior. We find the lattice responds linearly to stress in all cases, oblivious to the macroscopic unrecoverable strains, curvature, and hysteresis, localizing these effects to the contacts. Neutron diffraction shows that the more granular rocks appear to distribute stresses so that the same strain appears in all the grains, independent of crystallographic orientation.

A high-temperature tensile stress study of a monolithic silicon nitride (Si3N4) was performed with time-of-flight neutron diffraction. A dedicated engineering diffractometer was employed at temperatures reaching 1375 °C. Rietveld refinements of diffraction spectra allowed the determination of (1) the coefficient of thermal expansion tensor during heating and (2) lattice strains during loading. The stress–strain response of individual lattice reflections was used to calculate the single-crystal elastic stiffness tensor of Si3N4 at 1375 °C via a self-consistent model.

A high-temperature tensile stress study of a monolithic silicon nitride (Si3N4) was performed with time-of-flight neutron diffraction. A dedicated engineering diffractometer was employed at temperatures reaching 1375 °C. Rietveld refinements of diffraction spectra allowed the determination of (1) the coefficient of thermal expansion tensor during heating and (2) lattice strains during loading. The stress–strain response of individual lattice reflections was used to calculate the single-crystal elastic stiffness tensor of Si3N4 at 1375 °C via a self-consistent model.

We use hydrostatic pressure as an instrument to reveal a strong nonlinearity of the electrical polarization in group‐III nitride quantum well structures. From the photoluminescence peak energies of the quantum well emission at different applied pressures we obtain the values of the built‐in electric field in the wells and the corresponding well‐barrier polarization difference. We found that in both the InGaN/GaN and GaN/AlGaN systems the field and the polarization difference increase with pressure much faster than expected from the conventional (linear) model of polarization. This behavior is explained by the dramatic strain dependence of the piezoelectric coefficients of the group‐III nitrides, which constitutes the nonlinear piezoelectric effect.

In situ uniaxial compression experiments on Pb(Zr,Ti)O3 or PZT-based polycrystalline electroceramics were conducted using time-of-flight neutron diffraction. Elastic lattice strain and texture evolution were observed in PZT’s near the edge of the morphotropic phase boundary (with tetragonal and rhombohedral phases present). Multiphase Rietveld analysis yielded anisotropic lattice strain evolution curves in directions parallel and perpendicular to the loading axis for both phases. A quantitative analysis of the domain switching under applied stress was possible through application of a March–Dollase model for texture.

In situ uniaxial compression experiments on Pb(Zr,Ti)O3 or PZT-based polycrystalline electroceramics were conducted using time-of-flight neutron diffraction. Elastic lattice strain and texture evolution were observed in PZT’s near the edge of the morphotropic phase boundary (with tetragonal and rhombohedral phases present). Multiphase Rietveld analysis yielded anisotropic lattice strain evolution curves in directions parallel and perpendicular to the loading axis for both phases. A quantitative analysis of the domain switching under applied stress was possible through application of a March–Dollase model for texture.

The reduction of a solid NiAl2O4 cylinder to a metal-ceramic composite consisting of Ni particles in an Al2O3 matrix was monitored in situ at 1220 °C with neutron powder diffraction. The reaction kinetics was determined with a time resolution of 30 min. The reduction is associated with a volume shrinkage. A comparison of finite element calculations and the changes in the measured lattice parameters suggests that creep has relaxed the residual strains that would otherwise result from the volume shrinkage. The data also indicate that structural evolution in unreduced NiAl2O4 via a change in the cationic sublattice towards inverse spinel occurred and that led to a variation in lattice parameters.

The reduction of a solid NiAl2O4 cylinder to a metal-ceramic composite consisting of Ni particles in an Al2O3 matrix was monitored in situ at 1220 °C with neutron powder diffraction. The reaction kinetics was determined with a time resolution of 30 min. The reduction is associated with a volume shrinkage. A comparison of finite element calculations and the changes in the measured lattice parameters suggests that creep has relaxed the residual strains that would otherwise result from the volume shrinkage. The data also indicate that structural evolution in unreduced NiAl2O4 via a change in the cationic sublattice towards inverse spinel occurred and that led to a variation in lattice parameters.

Residual stresses generated by macroscopic inhomogeneous plastic deformation are predicted by an explicit finite element (FE) technique. The numerical predictions are evaluated by characterizing the residual elastic strains by neutron diffraction using two different ( hkl) reflections. Intergranular residual elastic strains between subsets of grains are predicted numerically and verified by neutron diffraction. Subsequently, the measured residual strain profiles in the test samples are modified by the intergranular strains and compared to the engineering predictions of the FE technique. Results compare well and verify the capability of the numerical technique as well as the possibilities of experimental validation using neutron diffraction. The presented experimental and numerical approach will subsequently be utilized for the evaluation of more complicated plastic deformation processes resembling forming operations.

Macrostrain variations in engineering components are frequently examined using neutron diffraction, at both reactors and pulsed sources. It is desirable to minimize the sampling volume in order to maximize the spatial resolution, although this increases the required measurement time. At reactors, macrostrain behavior is inferred from a single lattice reflection (deemed to be representative of the bulk response). At a pulsed source, a complete diffraction pattern is recorded and accordingly it is natural to fit the entire diffraction spectra using a Rietveld [J. Appl. Cryst. 2, 65 (1969)] refinement. This means that an idealized crystal structure is fit to the measured distorted crystal structure, which includes deviation of the measured lattice reflections from the ideal due to elastoplastic strain anisotropies, which are dependent on the particular lattice reflection (hkl) considered. We show that elastic macrostrains calculated from lattice parameter changes in Rietveld refinements (without accounting for hkl dependent anisotropies) are almost identical to the bulk elastic response and are comparable to the response obtained from a single lattice reflection typically used by practitioners at a steady state source. Moreover good refinements on the complete pattern are obtained with short measurement times compared to what is required for good statistics for single reflections. By incorporating a description of the elastic strain anisotropy expected in cubic materials into the Rietveld code, an empirical prediction of plastic strain history is possible. The validity of these arguments is demonstrated by analysis of a uniaxial tensile load test and a reanalysis of previously reported data taken on a deformed stainless steel ring. The plastic strain predictions compare favorably with a finite element model.