skip to main content
US FlagAn official website of the United States government
dot gov icon
Official websites use .gov
A .gov website belongs to an official government organization in the United States.
https lock icon
Secure .gov websites use HTTPS
A lock ( lock ) or https:// means you've safely connected to the .gov website. Share sensitive information only on official, secure websites.

Explore Research Products in the PAR
It may take a few hours for recently added research products to appear in PAR search results.


Title: Phase determination in dual phase steels via HREBSD‐based tetragonality mapping
Electron Backscatter Diffraction (EBSD) is a widely used approach for characterising the microstructure of various materials. However, it is difficult to accurately distinguish similar (body centred cubic and body centred tetragonal, with small tetragonality) phases in steels using standard EBSD software. One method to tackle the problem of phase distinction is to measure the tetragonality of the phases, which can be done using simulated patterns and cross‐correlation techniques to detect distortion away from a perfectly cubic crystal lattice. However, small errors in the determination of microscope geometry (the so‐called pattern or projection centre) can cause significant errors in tetragonality measurement and lead to erroneous results. This paper utilises a new approach for accurate pattern centre determination via a strain minimisation routine across a large number of grains in dual phase steels. Tetragonality maps are then produced and used to identify phase and estimate local carbon content. The technique is implemented using both kinetically simulated and dynamically simulated patterns to determine their relative accuracy. Tetragonality maps, and subsequent phase maps, based on dynamically simulated patterns in a point‐by‐point and grain average comparison are found to consistently produce more precise and accurate results, with close to 90% accuracy for grain phase identification, when compared with an image‐quality identification method. The error in tetragonality measurements appears to be of the order of 1%, thus producing a commensurate ∼0.2% error in carbon content estimation. Such an error makes the technique unsuitable for estimation of total carbon content of most commercial steels, which often have carbon levels below 0.1%. However, even in the DP steel for this study (0.1 wt.% carbon) it can be used to map carbon in regions with higher accumulation (such as in martensite with nonhomogeneous carbon content). Lay DescriptionElectron Backscatter Diffraction (EBSD) is a widely used approach for characterising the microstructure of various materials. However, it is difficult to accurately distinguish similar (BCC and BCT) phases in steels using standard EBSD software due to the small difference in crystal structure. One method to tackle the problem of phase distinction is to measure the tetragonality, or apparent ‘strain’ in the crystal lattice, of the phases. This can be done by comparing experimental EBSD patterns with simulated patterns via cross‐correlation techniques, to detect distortion away from a perfectly cubic crystal lattice. However, small errors in the determination of microscope geometry (the so‐called pattern or projection centre) can cause significant errors in tetragonality measurement and lead to erroneous results. This paper utilises a new approach for accurate pattern centre determination via a strain minimisation routine across a large number of grains in dual phase steels. Tetragonality maps are then produced and used to identify phase and estimate local carbon content. The technique is implemented using both simple kinetically simulated and more complex dynamically simulated patterns to determine their relative accuracy. Tetragonality maps, and subsequent phase maps, based on dynamically simulated patterns in a point‐by‐point and grain average comparison are found to consistently produce more precise and accurate results, with close to 90% accuracy for grain phase identification, when compared with an image‐quality identification method. The error in tetragonality measurements appears to be of the order of 1%, thus producing a commensurate error in carbon content estimation. Such an error makes an estimate of total carbon content particularly unsuitable for low carbon steels; although maps of local carbon content may still be revealing.Application of the method developed in this paper will lead to better understanding of the complex microstructures of steels, and the potential to design microstructures that deliver higher strength and ductility for common applications, such as vehicle components.  more » « less
Award ID(s):
1926662
PAR ID:
10488287
Author(s) / Creator(s):
; ; ; ; ;
Publisher / Repository:
Royal Microscopy Society
Date Published:
Journal Name:
Journal of Microscopy
Volume:
282
Issue:
1
ISSN:
0022-2720
Page Range / eLocation ID:
60 to 72
Format(s):
Medium: X
Sponsoring Org:
National Science Foundation
More Like this
  1. ; ; ; ; ; ; ; ; (, Ultramicroscopy)
    Electron backscatter diffraction (EBSD) is a powerful tool for determining the orientations of near-surface grains in engineering materials. However, many ceramics present challenges for routine EBSD data collection and indexing due to small grain sizes, high crack densities, beam and charge sensitivities, low crystal symmetries, and pseudo-symmetric pattern variants. Micro-cracked monoclinic hafnia, tetragonal hafnon, and hafnia/hafnon composites exhibit all such features, and are used in the present work to show the efficacy of a novel workflow based on a direct detecting EBSD sensor and a state-of-the-art pattern indexing approach. At 5 and 10 keV primary beam energies (where beam-induced damage and surface charge accumulation are minimal), the direct electron detector produces superior diffraction patterns with 10x lower doses compared to a phosphor-coupled indirect detector. Further, pseudo-symmetric variant-related indexing errors from a Hough-based approach (which account for at least 4%-14% of map areas) are easily resolved by dictionary indexing. In short, the workflow unlocks fundamentally new opportunities to characterize materials historically unsuited for EBSD. 
    more » « less
  2. ; ; ; ; ; (, Proceedings of the National Academy of Sciences)
    A ubiquitous structural feature in biological systems is texture in extracellular matrix that gains functions when hardened, for example, cell walls, insect scales, and diatom tests. Here, we develop patterned liquid crystal elastomer (LCE) particles by recapitulating the biophysical patterning mechanism that forms pollen grain surfaces. In pollen grains, a phase separation of extracellular material into a pattern of condensed and fluid-like phases induces undulations in the underlying elastic cell membrane to form patterns on the cell surface. In this work, LCE particles with variable surface patterns were created through a phase separation of liquid crystal oligomers (LCOs) droplet coupled to homeotropic anchoring at the droplet interface, analogously to the pollen grain wall formation. Specifically, nematically ordered polydisperse LCOs and isotropic organic solvent (dichloromethane) phase-separate at the surface of oil-in-water droplets, while, different LCO chain lengths segregate to different surface curvatures simultaneously. This phase separation, which creates a distortion in the director field, is in competition with homeotropic anchoring induced by sodium dodecyl sulfate (SDS). By tuning the polymer chemistry of the system, we are able to influence this separation process and tune the types of surface patterns in these pollen-like microparticles. Our study reveals that the energetically favorable biological mechanism can be leveraged to offer simple yet versatile approaches to synthesize microparticles for mechanosensing, tissue engineering, drug delivery, energy storage, and displays. 
    more » « less
  3. ; ; (, Journal of Geophysical Research: Solid Earth)
    Abstract To study the microstructural evolution of polymineralic rocks, we performed deformation experiments on two‐phase aggregates of olivine (Ol) + ferropericlase (Per) with periclase fractions (fPer) between 0.1 and 0.8. Additionally, single‐phase samples of both Ol and Per were deformed under the same experimental conditions to facilitate comparison of the microstructures in two‐phase and single‐phase materials. Each sample was deformed in torsion atT = 1523 K,P = 300 MPa at a constant strain rate up to a final shear strain of γ = 6 to 7. Microstructural developments, analyzed via electron backscatter diffraction (EBSD), indicate differences in both grain size and crystalline texture between single‐ and two‐phase samples. During deformation, grain size approximately doubled in our single‐phase samples of Ol and Per but remained unchanged or decreased in two‐phase samples. Zener‐pinning relationships fit to the mean grain sizes in each phase for samples with 0.1 ≤ fPer≤ 0.5 and for those with 0.8 ≥ fPer ≥ 0.5 demonstrate that the grain size of the primary phase is controlled by phase‐boundary pinning. Crystallographic preferred orientations, determined for both phases from EBSD data, are significantly weaker in the two‐phase materials than in the single‐phase materials. 
    more » « less
  4. ; ; ; ; (, Microstructures)
    Precession electron diffraction (PED) is a powerful technique for revealing the crystallographic orientation of samples at the nanoscale. However, the quality of orientation indexing is strongly influenced by the quality of diffraction patterns. In this study, we have developed a novel algorithm called Auto-CLAHE (automatic contrast-limited adaptive histogram equalization), which automatically enhances low-intensity diffraction pattern signals using contrast-limited adaptive histogram equalization (CLAHE). The degree of enhancement is dynamically adjusted based on the overall intensity of the diffraction pattern, with greater enhancement applied to patterns with fewer spots (i.e., away from zone axes) and little or no enhancement applied to patterns with many spots (i.e., at a zone axis). By improving the visibility of low-intensity diffraction spots, Auto-CLAHE significantly improves the template matching between experimentally acquired and simulated diffraction patterns, leading to orientation maps with dramatically higher quality and lower noise. We anticipate that Auto-CLAHE provides an efficient and practical solution for preprocessing PED data, enabling higher-quality crystal orientation mapping to be routinely obtained. 
    more » « less
  5. ; ; ; (, IMA Journal of Applied Mathematics)
    null (Ed.)
    Abstract Non-topological defects in spatial patterns such as grain boundaries in crystalline materials arise from local variations of the pattern properties such as amplitude, wavelength and orientation. Such non-topological defects may be treated as spatially localized structures, i.e. as fronts connecting distinct periodic states. Using the two-dimensional quadratic-cubic Swift–Hohenberg equation, we obtain fully nonlinear equilibria containing grain boundaries that separate a patch of hexagons with one orientation (the grain) from an identical hexagonal state with a different orientation (the background). These grain boundaries take the form of closed curves with multiple penta-hepta defects that arise from local orientation mismatches between the two competing hexagonal structures. Multiple isolas occurring robustly over a wide range of parameters are obtained even in the absence of a unique Maxwell point, underlining the importance of retaining pinning when analysing patterns with defects, an effect omitted from the commonly used amplitude-phase description. Similar results are obtained for quasiperiodic structures in a two-scale phase-field model. 
    more » « less
  • Citation Formats
  • MLA
  • APA
  • Chicago
  • BibTeX
  • Save / Share this Record
  • Send to Email