Three dimensional strain measurements with x-ray energy dispersive spectroscopy

Black, David R.; Bechtoldt, C. J.; Placious, R. C.; Kuriyama, M.

doi:10.1007/bf00568760

Cited by 20 publications

(10 citation statements)

References 2 publications

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“…The profile resolution is affected by the angular divergence of the incident beam and is thus able to detect tiny changes in the crystal structures of Li x Ni 1/3 Co 1/3 Mn 1/3 O 2 at the different SOC. In general, the profile resolution (i.e., Δd/d) of the EDXRD is composed of the angular divergence of the X-ray beam (Δθ) and the energy resolution of monochromating device, e.g., energy-discriminating detector 15 and monochromator, (ΔE) as follows:…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

Spectroscopic X-ray Diffraction for Microfocus Inspection of Li-Ion Batteries

et al. 2014

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We developed spectroscopic X-ray diffraction (XRD) analysis to visualize electrochemical reactions occurring at various locations in Li-ion batteries (LIBs). Continuous irradiation with monochromatic X-rays in an energy region using a confocal setup provided a fixed observation position on the order of several tens of microns. Unlike three-dimensionally position sensitive XRD analyses, e.g., angle-scanning XRD and energydispersive XRD, this energy-scanning XRD analysis with angle-scanning of the monochromator instead of the detector-scanning has the advantage of profile resolution, position sensitivity, and time-resolution for mapping concentration gradients and diffusion of Li + associated with the electrochemical properties of LIBs. The microscopic structural inhomogeneity in a sheet-like composite electrode of LiNi 1/3 Co 1/3 Mn 1/3 O 2 with a thickness of 150 μm was successfully determined with a depth resolution of 50 μm during cell operation. This work demonstrates the potential of spectroscopic XRD as a nondestructive and pinpoint analysis method, thus contributing to the development of high-performance LIBs. ■ INTRODUCTIONLi-ion batteries (LIBs) have been extensively used in portable electronics, including laptop computers and mobile phones. 1−3 Owing to strong, increasing demands in the automotive field, 4,5 further improvements in power density are expected. The properties of LIBs, including energy density, capacity, response, and cycle life, are primarily governed by their electrical and ionic conductive networks. 6−8 Most LIBs consist of versatile composite electrodes containing active materials, conductive agents, and binders coated on current collectors to promote smooth Li + communication. However, this complex structure complicates an understanding of the inevitable microscopic inhomogeneities in the spatial variations of the Li + concentration, i.e., the unreactive portion. Therefore, elucidating the mechanism by which inhomogeneities occur in the composite electrode during operation is critical for the development of LIBs. To visualize these kinetic phenomena in complex systems, advanced analyses must be developed.Electrochemical reactions occurring at the composite electrode have been intensively investigated by a variety of in situ techniques such as spectroscopic, microscopic, and diffractometric methods. 9−11 In particular, the diffraction techniques using hard X-rays offer useful information on the Li + concentration in the crystalline samples as a lattice constant and, thus, a state of charge (SOC) of a LIB can be understood by differences not only in the overall electron flow but also in the bulk crystal structure. 12−14 These differences motivated us to develop a rapid and high-resolution X-ray diffraction (XRD) imaging technique to map electrochemical reactions based on a novel concept. In the conventional angle-scanning XRD method, the detector angle is varied to detect a series of elastic scatterings diffracted from the sample, resulting in geometrical changes in the X-ray probe area....

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Section: ■ Experimental Sectionmentioning

confidence: 99%

Spectroscopic X-ray Diffraction for Microfocus Inspection of Li-Ion Batteries

et al. 2014

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“…For the progress made in the first decade after the introduction of the ED method the reader is referred to the bibliography compiled by Laine & Lä hteenmä ki (1980). Concerning X-ray stress analysis (XSA) the first applications of white-beam diffraction using commercially available X-ray sources were reported in the late 1970s (Nagao & Kusumoto, 1977) and the early 1980s (Bechtoldt et al, 1982;Black et al, 1985). The main advantage of ED diffraction experiments compared to AD diffraction is the simple experimental setup.…”

Section: Introductionmentioning

confidence: 99%

Energy-dispersive diffraction stress analysis under laboratory and synchrotron conditions: a comparative study

et al. 2010

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For a feasibility study of energy‐dispersive residual stress analysis under laboratory conditions, an X‐ray diffractometer that has been operated so far in the angle dispersive diffraction mode was equipped with a commercial tungsten tube and an energy‐dispersive solid‐state germanium detector. Starting from systematic investigations to find the optimum configuration regarding geometrical resolution, measuring time and stability of the applied detector system, different materials were characterized with respect to the near‐surface residual stress state. The results achieved with the modified laboratory equipment within reasonable measuring times are in good agreement with synchrotron measurements performed on the same samples. With the example of a shot‐peened Al2O3 ceramic with a highly non‐uniform near‐surface residual stress distribution it is furthermore shown that the different size and shape of the diffracting gauge volume used for the laboratory and synchrotron measurements might have a significant influence on the experimentally obtained Laplace‐space residual stress depth profiles σ||(τ).

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“…Residual stress techniques using white radiation have been attempted and published. [11,[14][15][16] Compared to the conventional method (single wavelength, moving detector), energy dispersive diffraction is faster because the entire diffraction peak or peaks are determined simultaneously. However, the method suffers from poor accuracy for several reasons:…”

Section: Determination Of Practical Radiationsmentioning

confidence: 99%

Development of Nondestructive Residual Stress Profile Measurement Methods — The Integral Method

Hornbach¹,

Prevéy²,

Blodgett³

2005

AIP Conference Proceedings

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A modified Integral Method was investigated as a means to nondestructively measure the subsurface residual stress distribution. The technique has been demonstrated to be feasible in aluminum alloys by comparison to established destructive measurement methods. In the current effort a thorough study of higher energy radiations was conducted to obtain deeper penetrating radiations on titanium and nickel base alloys. Higher energy radiation used in conjunction with the modified Integral Method would provide nondestructive subsurface residual stress measurement in components composed of these alloys.

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Three dimensional strain measurements with x-ray energy dispersive spectroscopy

Cited by 20 publications

References 2 publications

Spectroscopic X-ray Diffraction for Microfocus Inspection of Li-Ion Batteries

Spectroscopic X-ray Diffraction for Microfocus Inspection of Li-Ion Batteries

Energy-dispersive diffraction stress analysis under laboratory and synchrotron conditions: a comparative study

Development of Nondestructive Residual Stress Profile Measurement Methods — The Integral Method

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