Hemant Sharma

A fast methodology to determine the characteristics of thousands of grains using three-dimensional X-ray diffraction. I. Overlapping diffraction peaks and parameters of the experimental setup

A data-analysis methodology is presented for the characterization of three-dimensional microstructures of polycrystalline materials from data acquired using three-dimensional X-ray diffraction (3DXRD). The method is developed for 3DXRD microscopy using a far-field detector and yields information about the centre-of-mass position, crystallographic orientation, volume and strain state for thousands of grains. This first part deals with pre-processing of the diffraction data for input into the algorithms presented in the second part [Sharma, Huizenga & Offerman (2012). J. Appl. Cryst. 45, 705–718] for determination of the grain characteristics. An algorithm is presented for accurate identification of overlapping diffraction peaks from X-ray diffraction images, which has been an issue limiting the accuracy of experiments of this type. The algorithm works in two stages, namely the identification of overlapping peaks using a seeded watershed algorithm, and then the fitting of the peaks with a pseudo-Voigt shape function to yield an accurate centre-of-mass position and integrated intensity for the peaks. Regions consisting of up to six overlapping peaks can be successfully fitted. Two simulations and an experiment are used to verify the results of the algorithms. An example of the processing of diffraction images acquired in a 3DXRD experiment with a sample consisting of more than 1600 grains is shown. Furthermore, a procedure for the determination of the parameters of the experimental setup (global parameters) without the need for a calibration sample is presented and validated using simulations. This is immensely beneficial for simplifying experiments and the subsequent data analysis.

Multipurpose furnace for in situ studies of polycrystalline materials using synchrotron radiation

We report a multipurpose furnace designed for studies using synchrotron radiation on polycrystalline materials, namely, metals, ceramics, and (semi)crystalline polymers. The furnace has been designed to carry out three-dimensional (3D) x-ray diffraction measurements but can also be used for other types of synchrotron radiation research. The furnace has a very low thermal gradient across the specimen (<0.2 degrees C/mm). Accurate determination of the temperature can be carried out by welding a thermocouple to the specimen. The furnace can be rotated over an angle of 90 degrees in order to determine the crystallographic orientation of each individual grain. It is possible to follow growth kinetics of all grains in the illuminated volume of the specimen. The specimen environment can be controlled varying from vacuum (up to 10(-5) mbar) to gas or air filled. The maximum temperature of operation is 1500 degrees C, with the possibility of achieving high heating (up to 20 degrees C/s) and cooling rates (up to 30 degrees C/s without quenching gas). 3D maps of the microstructure of the specimen can be generated at elevated temperatures by bringing the high-resolution detector close to the specimen. We show an example of a simulation of the heat affected zone during the thermal cycle of a weld in a transformation-induced plasticity steel carried out using the furnace. The unique characteristics of the furnace open possibility of new fields in materials research using synchrotron radiation.

Influences of granular constraints and surface effects on the heterogeneity of elastic, superelastic, and plastic responses of polycrystalline shape memory alloys

Abstract Deformation heterogeneities at the microstructural length-scale developed in polycrystalline shape memory alloys (SMAs) during superelastic loading are studied using both experiments and simulations. In situ X-ray diffraction, specifically the far-field high energy diffraction microscopy (ff-HEDM) technique, was used to non-destructively measure the grain-averaged statistics of position, crystal orientation, elastic strain tensor, and volume for hundreds of austenite grains in a superelastically loaded nickel-titanium (NiTi) SMA. These experimental data were also used to create a synthetic microstructure within a finite element model. The development of intragranular stresses were then simulated during tensile loading of the model using anisotropic elasticity. Driving forces for phase transformation and slip were calculated from these stresses. The grain-average responses of individual austenite crystals examined before and after multiple stress-induced transformation events showed that grains in the specimen interior carry more axial stress than the surface grains as the superelastic response “shakes down”. Examination of the heterogeneity within individual grains showed that regions near grain boundaries exhibit larger stress variation compared to the grain interiors. This intragranular heterogeneity is more strongly driven by the constraints of neighboring grains than the initial stress state and orientation of the individual grains.

Formation of (Fe,Cr) carbides and dislocation structures in low-chromium steel studied in situ using synchrotron radiation

The evolution of the size distribution of (Fe,Cr) carbides and the dislocation structure in low-chromium steel is studied during quenching and rapid heating by in situ small-angle X-ray scattering (SAXS). The two-dimensional SAXS patterns consist of streaks on top of an isotropic SAXS signal. The evolution of the size distribution of the (Fe,Cr) carbides during heat treatment is determined from the isotropic component of the SAXS patterns. The isotropic part of the SAXS patterns shows that, after austenitization and quenching to room temperature, the average precipitate radius is 4.74 nm and the dispersion parameter for the lognormal size distribution is 0.33. Subsequent rapid heating to 823 K results in an average precipitate size of 5.25 nm and a dispersion parameter of 0.26. Bright-field transmission electron microscopy and high-resolution transmission electron microscopy reveal the nearly spherical morphology of the precipitates. The microstructural evolution underlying the increase in the average precipitate size and the decrease in the dispersion parameter after heating to and annealing at 823 K is probably that at room temperature two types of precipitates are present, i.e. (Fe,Cr)23C6 and (Fe,Cr)7C3 precipitates according to thermodynamic calculations, and at 823 K only (Fe,Cr)7C3 precipitates are present. Additional measurements have been carried out on a single crystal of ferrite containing (Fe,Cr) carbides by combining three-dimensional X-ray diffraction (3DXRD) and SAXS during rotation of the specimen at room temperature, in order to investigate the origin of the streaks at low angles in the SAXS pattern. From simulations based on the theory of SAXS from dislocations, it is shown that the measured streaks, including the spottiness, in the two-dimensional SAXS patterns correspond to a dislocation structure of symmetric low-angle tilt boundaries, which in turn corresponds to the crystallographic orientation gradient in the single crystal of ferrite as measured by 3DXRD microscopy.

Big Data Staging with MPI-IO for Interactive X-ray Science

New techniques in X-ray scattering science experiments produce large data sets that can require millions of high-performance processing hours per week of computation for analysis. In such applications, data is typically moved from X-ray detectors to a large parallel file system shared by all nodes of a peta scale supercomputer and then is read repeatedly as different science application tasks proceed. However, this straightforward implementation causes significant contention in the file system. We propose an alternative approach in which data is instead staged into and cached in compute node memory for extended periods, during which time various processing tasks may efficiently access it. We describe here such a big data staging framework, based on MPI-IO and the Swift parallel scripting language. We discuss a range of large-scale data management issues involved in X-ray scattering science and measure the performance benefits of the new staging framework for high-energy diffraction microscopy, an important emerging application in data-intensive X-ray scattering. We show that our framework accelerates scientific processing turnaround from three months to under 10 minutes, and that our I/O technique reduces input overheads by a factor of 5 on 8K Blue Gene/Q nodes.

Eliminating the non-Gaussian spectral response of X-ray absorbers for transition-edge sensors

Transition-edge sensors (TESs) as microcalorimeters for high-energy-resolution X-ray spectroscopy are often fabricated with an absorber made of materials with high Z (for X-ray stopping power) and low heat capacity (for high resolving power). Bismuth represents one of the most compelling options. TESs with evaporated bismuth absorbers have shown spectra with undesirable and unexplained low-energy tails. We have developed TESs with electroplated bismuth absorbers over a gold layer that are not afflicted by this problem and that retain the other positive aspects of this material. To better understand these phenomena, we have studied a series of TESs with gold, gold/evaporated bismuth, and gold/electroplated bismuth absorbers, fabricated on the same die with identical thermal coupling. We show that the bismuth morphology is linked to the spectral response of X-ray TES microcalorimeters.

Grain Nucleation and Growth of Individual Austenite and Ferrite Grains Studied by 3DXRD Microscopy at the ESRF

The mechanical properties of steel strongly depend on the microstructure, which is formed during the production and processing of steel. Understanding the underlying mechanisms of the nucleation and growth kinetics during solid-state phase transformations in steel is of vital importance to control the microstructure of steel. The kinetics of individual grains in the bulk of steel can be measured in situ with the three-dimensional X-ray diffraction microscopy (3DXRD) at the European synchrotron radiation facility (ESRF). Simultaneously the fraction transformed, the nucleation rate, and the growth rate of individual grains can be measured. A furnace was developed to match with the 3DXRD-technology with the aim to map the three-dimensional microstructure of steel at elevated temperatures and to follow the kinetics of individual grains in more detail. Unique in situ measurements of nucleation and growth rates of individual austenite and ferrite grains are presented.

In-line x-ray phase-contrast tomography and diffraction-contrast tomography study of the ferrite-cementite microstructure in steel

This work presents the development of a non-destructive imaging technique for the investigation of the microstructure of cementite grains embedded in a ferrite matrix of medium-carbon steel. The measurements were carried out at the material science beamline of the European Synchrotron Radiation Facility (ESRF) ID11. It was shown that in-line X-ray phase-contrast tomography (PCT) can be used for the detection of cementite grains of several microns in size. X-ray PCT of the cementite structure can be achieved by either a ‘single distance’ or a ‘multiple distance’ acquisition protocol. The latter permits quantitative phase retrieval. A second imaging technique, X-ray diffraction-contrast tomography (DCT), was employed to obtain information about the shapes and crystallographic orientations of the distinct ferrite grains surrounding the cementite structures. The initial results demonstrate the feasibility of determining the geometry of the cementite grains after the austenite-ferrite phase-transformation in a non-destructive manner. The results obtained with PCT and DCT are verified with ex-situ optical microscopy studies of the same specimen.

Microstructure Analysis of Bismuth Absorbers for Transition-Edge Sensor X-ray Microcalorimeters

Given its large X-ray stopping power and low specific heat capacity, bismuth (Bi) is a promising absorber material for X-ray microcalorimeters and has been used with transition-edge sensors (TESs) in the past. However, distinct X-ray spectral features have been observed in TESs with Bi absorbers deposited with different techniques. Evaporated Bi absorbers are widely reported to have non-Gaussian low-energy tails, while electroplated ones do not show this feature. In this study, we fabricated Bi absorbers with these two methods and performed microstructure analysis using scanning electron microscopy and X-ray diffraction microscopy. The two types of material showed the same crystallographic structure, but the grain size of the electroplated Bi was about 40 times larger than that of the evaporated Bi. This distinction in grain size is likely to be the cause of their different spectral responses.

Practices and Standards for Data and Processing at the APS

The handling of datasets at scientific user facilities is becoming progressively more challenging as advances in sources and detectors drive increasingly aggressive data acquisition rates. The ability to share and process these data depends on the ability of the originator of the data and the persons making use of that data to unequivocally agree on what these data mean. This understanding is driven by use of standardized data formats.