DOI: 10.5281/zenodo.7311323
title: Synchrotron X-ray Diffraction Analysis - Measuring Bulk Crystallographic Texture from Differently-Orientated Ti-6Al-4V Samples

description: A dataset of synchrotron X-ray diffraction (SXRD) analysis files, recording the refinement of crystallographic texture from six differently orientated Ti-6Al-4V (Ti-64) samples. Two different refinement methods were used to fit a range of diffraction pattern ring intensities, for determining crystallographic texture in both α (hexagonal close packed, hcp) and β (body-centred cubic, bcc) phases. The first procedure was based on an established Rietveld refinement method, using the software package MAUD (Materials Analysis Using Diffraction). The second procedure uses a new Fourier-based peak fitting method from the Continuous-Peak-Fit Python package. Both methods were used to calculate texture from each of the six different sample orientations, a combination of the six sample orientations, and in a batch processing method for calculating spatially-resolved texture variation from 387 individual X-Y stage-scan SXRD measurements across one of the samples. <strong>Material</strong> The Ti-64 material used in this study was pre-rolled to 87.5% reduction at 915ºC and then air-cooled to develop a characteristic texture. Six different rectangular samples were cut from this material and are referenced according to alignment with the original rolling directions (RD – rolling direction, TD – transverse direction, ND – normal direction), and alignment with the horizontal (X) and vertical (Y) axes of the synchrotron detector; A table recording the SXRD run number and sample orientation analysed. <em>Run Number</em> <em>Sample Orientation Reference</em> <em>Sample Orientation (Horizontal - Vertical)</em> 103840 Sample 6 TD45ºRD - ND 103841 Sample 5 RD - TD45ºND 103842 Sample 4 TD - RD45ºND 103843 Sample 3 RD - TD 103844 Sample 2 RD - ND 103845 Sample 1 TD - ND <strong>Diffraction Pattern Averaging </strong> The .cbf images found in the raw dataset were first converted into .tiff images. The stage-scan images were then averaged together for each of the different sample orientations, using a Python notebook sxrd-tiff-summer, to produce six averaged .tiff images. These averaged .tiff image capture average diffraction peak intensities from an area of about 96.75 mm<sup>2</sup> (equivalent to a total volume of around 193.5 mm<sup>3</sup>) from each piece, which is therefore representative of bulk crystallographic texture from six different sample orientations. <strong>MAUD Analysis </strong> To process data using MAUD the diffraction pattern images must first be caked, which converts the data into .dat files of intensity versus 2θ profiles, using 72 azimuthal cakes, each of 5° azimuthal width. Although MAUD has an in-built function to cake data, using ImageJ, it is not possible to cake data in MAUD with ImageJ in an automated way. Therefore, caking was done using pyFAI, an open-source Python package, with the caking procedure recorded in a separate Python notebook, pyFAI-integration-caking. The caking was applied to each of the six averaged tiff images, as well as being applied to 387 individual X-Y stage-scan tiff images from Sample 1 (103845). The caking procedure was also applied to the CeO2 calibrant diffraction pattern, creating a .dat file that could be used for calibration of the instrument parameters within MAUD, before fitting the experimental data from the different samples. A separate package MAUD-batch-analysis was used to record the setup of the files and details of the refinement procedure. Details about the refinement procedure are also recorded in an accompanying paper reporting on these results. A number of refinement steps were used to fit the caked data from the six different sample orientations, and calculate texture. Texture was also calculated from a .dat file that combined all six sample orientations together. The crystallographic texture was refined using the E-WIMV algorithm, which was found to best reproduce quantitative texture intensity values with an orientation distribution function (ODF) resolution of 15º. The MAUD-batch-analysis package also contains details about how to setup and run MAUD in an automated batch processing mode. MAUD's batch mode was used to calculate texture from a series of 387 individual stage-scan diffraction patterns from Sample 1 (103845). A MAUD-batch-analysis script was first used to substitute caked data from the 387 diffraction patterns into template .par files, which contained an initial refinement of the volume fraction, crystal sizes and micro-strain, as a starting point. Both the crystal parameters and texture were then iteratively refined, in MAUD, using a .ins batch analysis script launched from the terminal. This was done to refine both α and then β phase texture. The texture data from the MAUD analysis was recorded as an ODF, with 15º resolution over all Euler space, and extracted in text format using a script from MAUD-batch-analysis. These text files can be loaded into MTEX, for plotting and analysing both the α and β phase crystallographic texture. <strong>Continuous-Peak-Fit Analysis </strong> A .poni calibration file was created using Dioptas, through a refinement matching peak intensities from a CeO2 standard diffraction pattern image. Dioptas was then used to determine peak bounds in 2θ for characterising a total of 21 α and 4 β lattice plane rings from the Ti-64 diffraction pattern images, which were recorded in a .py input script. Using these two inputs, Continuous-Peak-Fit automatically converts full diffraction pattern rings into profiles of intensity versus azimuthal angle, for each 2θ section, which can also include multiple overlapping α and β peaks. The Continuous-Peak-Fit refinement can then be launched in a notebook or from the terminal, to automatically calculate a full mathematical description, in the form of Fourier expansion terms, to match the intensity variation of each individual lattice plane ring. The results for peak position, intensity and half-width for all 21 α and 4 β lattice plane peaks were recorded at an azimuthal resolution of 1º and stored in a .fit output file. Details for setting up and running this analysis can be found in the continuous-peak-fit-analysis package. This package also includes a Python script for extracting lattice plane ring intensity distributions from the .fit files, matching the intensity values with spherical polar coordinates to parametrise the intensity distributions from each of the six different sample orientations, in the form of pole figures. The script can also be used to combine intensity distributions from different sample orientations. The final intensity variations are recorded for each of the lattice plane peaks as text files, which can be loaded into MTEX to plot and analyse both the α and β phase crystallographic texture. This method was also used to analyse all 387 individual diffraction patterns recorded across Sample 1 (S1 – 103845), to quantify the texture variation across the piece. <strong>Metadata </strong> An accompanying YAML text file contains associated processing metadata for both the MAUD and the Continuous-Peak-Fit analyses, recording information about the different packages used to process the data, along with details about the different files contained within this analysis dataset.