Special Issue "In Situ X-Ray Diffraction on Metals and Alloys"

A special issue of Metals (ISSN 2075-4701).

Deadline for manuscript submissions: closed (31 May 2019)

Special Issue Editor

Guest Editor
Dr. Guillaume Geandier

Institut Jean Lamour, CNRS - Université de Lorraine, Campus Artem, 2 allée André Guinier, BP 50840, 54011 Nancy Cedex, France
Website | E-Mail
Interests: microstructure; strain-stress; internal stresses; in situ X-rays diffraction; phase transformation; synchrotron

Special Issue Information

Dear Colleagues,

With new-generation diffractometers, detectors and synchrotron sources, it is time to focus our research on metals and alloys developed with in situ X-rays methods.

The aim is to describe several kinds of results using original devices that have been developed in laboratories or specially designed for synchrotron beamlines. Results will form a large part of this Special Issue, but some focus is needed on the specificities of the sample environment due to the specificities of the metallic samples and their interaction with X-rays (high absorption, fast or low kinetics of the studied phenomena, etc.) and also the work to be done with the data. In situ analysis means a lot of data to analyze with several constraints (large volume, synchronization of signals, evolution of the sample, multiple analysis, statistics, …)

The main idea of this particular issue is to show the impressive results that can be obtained using in situ X-rays; the work that needs to be done to design (or even use) a sample environment adapted to metals and alloys analysis; the time and work required for data extracted from the complete device.

Dr. Geandier Guillaume
Guest Editor

Manuscript Submission Information

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Keywords

  • In situ X-rays
  • Sample environment
  • Data analysis
  • Metals
  • Metallic alloys

Published Papers (4 papers)

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Research

Open AccessArticle
Advanced Non-Destructive in Situ Characterization of Metals with the French Collaborating Research Group D2AM/BM02 Beamline at the European Synchrotron Radiation Facility
Metals 2019, 9(3), 352; https://doi.org/10.3390/met9030352
Received: 27 February 2019 / Revised: 8 March 2019 / Accepted: 14 March 2019 / Published: 19 March 2019
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Abstract
The ability to non-destructively measure the structural properties of devices, either in situ or operando, are now possible using an intense X-ray synchrotron source combined with specialized equipment. This tool attracted researchers, in particular metallurgists, to attempt more complex and ambitious experiments aimed [...] Read more.
The ability to non-destructively measure the structural properties of devices, either in situ or operando, are now possible using an intense X-ray synchrotron source combined with specialized equipment. This tool attracted researchers, in particular metallurgists, to attempt more complex and ambitious experiments aimed at answering unresolved questions in formation mechanisms, phase transitions, and magnetism complex alloys for industrial applications. In this paper, we introduce the diffraction diffusion anomale multi-longueur d’onde (D2AM) beamline, a French collaborating research group (CRG) beamline at the European Synchrotron Radiation Facility (ESRF), partially dedicated to in situ X-ray scattering experiments. The design of the beamline combined with the available equipment (two-dimensional fast photon counting detectors, sophisticated high precision kappa diffractometer, a variety of sample environments, continuous scanning for X-ray imaging, and specific software for data analysis) has made the D2AM beamline a highly efficient tool for advanced, in situ synchrotron characterization in materials science, e.g., single crystal or polycrystalline materials, powders, liquids, thin films, or epitaxial nanostructures. This paper gathers the main elements and equipment available at the beamline and shows its potential and flexibility in performing a wide variety of temporally, spatially, and energetically resolved X-ray synchrotron scattering measurements in situ. Full article
(This article belongs to the Special Issue In Situ X-Ray Diffraction on Metals and Alloys)
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Open AccessArticle
Real-Time Investigation of Recovery, Recrystallization and Austenite Transformation during Annealing of a Cold-Rolled Steel Using High Energy X-ray Diffraction (HEXRD)
Received: 26 November 2018 / Revised: 16 December 2018 / Accepted: 19 December 2018 / Published: 21 December 2018
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Abstract
The annealing process of cold-rolled ferrite/pearlite steel involves numerous metallurgical mechanisms as recovery/recrystallization of deformed phases, ripening of carbide microstructure, and austenite transformation in the intercritical domain. The interactions between these mechanisms govern the morphogenesis of the transformed austenite microstructure and, thus, the [...] Read more.
The annealing process of cold-rolled ferrite/pearlite steel involves numerous metallurgical mechanisms as recovery/recrystallization of deformed phases, ripening of carbide microstructure, and austenite transformation in the intercritical domain. The interactions between these mechanisms govern the morphogenesis of the transformed austenite microstructure and, thus, the final properties of the steel. This paper demonstrates that high energy X-ray diffraction (HEXRD) on synchrotron beamline offers the unique possibility to follow concomitantly these mechanisms in situ during a single experiment. A cold-rolled ferrite-pearlite steel dedicated to the industrial production of Dual-Phase steel serves as case-study. Synchrotron experiments have been conducted in transmission at 100 keV with a 2D detector. Diffraction patterns acquired all along an annealing treatment are first analyzed after circular integration. A Rietveld refinement procedure coupled with a Williamson-Hall approach is used to determine phase transformation and recovery kinetics. In this paper, a new method inspired by the 3D X-ray diffraction tomography is proposed to follow recrystallization kinetics at the same time. It is based on a systematic detection of individual diffraction spots related to newly recrystallized grains appearing on Debye-Scherrer rings. The deduced recrystallization kinetics is compared and validated by more conventional ex situ methods. Full article
(This article belongs to the Special Issue In Situ X-Ray Diffraction on Metals and Alloys)
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Graphical abstract

Open AccessArticle
Determination of Residual Stresses in an Oxidized Metallic Alloy under Thermal Loadings
Metals 2018, 8(11), 913; https://doi.org/10.3390/met8110913
Received: 28 August 2018 / Revised: 3 October 2018 / Accepted: 27 October 2018 / Published: 6 November 2018
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Abstract
In order to clarify the mechanical features of a metal under thermal cyclic loading for the system Ni30Cr-Cr2O3, a specific study has been carried out. In the present work, the residual stresses in both the metal and the [...] Read more.
In order to clarify the mechanical features of a metal under thermal cyclic loading for the system Ni30Cr- Cr 2 O 3 , a specific study has been carried out. In the present work, the residual stresses in both the metal and the oxide layer have been investigated. An adapted method is applied to process the experimental results that were obtained by using in-situ high temperature synchrotron diffraction at European Synchrotron Radiation Facility. The sin 2 ψ analysis provides information about the stress in metal and oxide. X-ray diffraction provides also the lattice parameter between crystallographic planes in the metal. To obtain correct stress values, a correction method is also proposed taking into account different discrepancies sources to ensure the equation of mechanical balance. Full article
(This article belongs to the Special Issue In Situ X-Ray Diffraction on Metals and Alloys)
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Figure 1

Open AccessArticle
A Study on the Nanoparticles Evolution in Isothermally Aged Strain Glass of Ti48.7Ni51.3 Shape Memory Alloy by In Situ Small-Angle X-ray Scattering
Metals 2018, 8(5), 352; https://doi.org/10.3390/met8050352
Received: 6 March 2018 / Revised: 20 April 2018 / Accepted: 11 May 2018 / Published: 14 May 2018
Cited by 1 | PDF Full-text (3633 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Ni-rich nanodomains and Ti3Ni4 nanoprecipitates in the strain glass of Ni-rich Ti-Ni shape memory alloys (SMAs) play an important role in the origin and characteristic control of the strain glass transition. Ni-rich nanodomains are formed in the quenching process and [...] Read more.
Ni-rich nanodomains and Ti3Ni4 nanoprecipitates in the strain glass of Ni-rich Ti-Ni shape memory alloys (SMAs) play an important role in the origin and characteristic control of the strain glass transition. Ni-rich nanodomains are formed in the quenching process and dissolve during isothermal aging. Ti3Ni4 nanoprecipitates nucleate, grow and coarsen during aging. This study performed in situ small-angle X-ray scattering (SAXS) and ex situ X-ray diffraction to investigate the structural evolutions with aging time of nanoparticles in Ti48.7Ni51.3 SMA aged isothermally at 250 °C in terms of relative volume fraction, radius, thickness, orientation, lattice ordering, and morphology. The mechanism and kinetics of the concurrent phase evolutions of Ni-rich nanodomains and Ti3Ni4 nanoprecipitates are revealed and discussed in detail. Frequency-dependent storage modulus vs. temperature at different frequencies for different aging times was measured to characterize the strain glass transition. Quantitative correlation of all structural evolutions and kinetics of Ni-rich and Ti3Ni4 nanoparticles with respect to the variation and loss of the strain glass transition during aging times of 0 to 20 h is presented. The roles of different nanoparticles in causing or suppressing the strain glass behavior are also experimentally revealed. Full article
(This article belongs to the Special Issue In Situ X-Ray Diffraction on Metals and Alloys)
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Graphical abstract

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