An operando spatially resolved study of alkaline battery discharge using a novel hyperspectral detector and X-ray tomography

An experimental technique is described for the collection of time-resolved X-ray diffraction information from a complete commercial battery cell during discharging or charging cycles. The technique uses an 80 × 80 pixel 2D energy-discriminating detector in a pinhole camera geometry which can be used with a polychromatic X-ray source. The concept was proved in a synchrotron X-ray study of commercial alkaline Zn–MnO2 AA size cells. Importantly, no modification of the cell was required. The technique enabled spatial and temporal changes to be observed with a time resolution of 20 min (5 min of data collection with a 15 min wait between scans). Chemical changes in the cell determined from diffraction information were correlated with complementary X-ray tomography scans performed on similar cells from the same batch. The clearest results were for the spatial and temporal changes in the Zn anode. Spatially, there was a sequential transformation of Zn to ZnO in the direction from the separator towards the current collector. Temporally, it was possible to track the transformation of Zn to ZnO during the discharge and follow the corresponding changes in the cathode.

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CHEMICAL DYNAMICS AND PHASE TRANSFORMATION IN HIGH TEMPERATURE PROCESSES USING TIME RESOLVED AND SPATIALLY RESOLVED X-RAY DIFFRACTION

Chemical Applications of Synchrotron Radiation - Advanced Series in Physical Chemistry ◽

10.1142/9789812775757_0020 ◽

2002 ◽

pp. 948-986 ◽

Cited By ~ 1

Author(s):

Joe Wong

Keyword(s):

Phase Transformation ◽

High Temperature ◽

Chemical Dynamics ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Spatially Resolved ◽

High Temperature Processes

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ChemInform Abstract: Chemical Dynamics and Phase Transformation in High Temperature Processes Using Time-Resolved and Spatially Resolved X-Ray Diffraction

ChemInform ◽

10.1002/chin.200246279 ◽

2010 ◽

Vol 33 (46) ◽

pp. no-no

Author(s):

Joe Wong

Keyword(s):

Phase Transformation ◽

High Temperature ◽

Chemical Dynamics ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Spatially Resolved ◽

High Temperature Processes

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In-Situ Chemical Dynamics and Phase Mapping Under Steep Thermal Gradients Using Time-Resolved and Spatially Resolved X-Ray Diffraction

Properties of Complex Inorganic Solids 2 ◽

10.1007/978-1-4615-1205-9_22 ◽

2000 ◽

pp. 285-306

Author(s):

Joe Wong ◽

E. M. Larson ◽

J. B. Holt ◽

T. Ressler ◽

J. W. Elmer

Keyword(s):

Thermal Gradients ◽

Chemical Dynamics ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Spatially Resolved ◽

Phase Mapping

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Direct observations of shock-induced melting in a porous solid using time-resolved x-ray diffraction

Physical Review Materials ◽

10.1103/physrevmaterials.4.063604 ◽

2020 ◽

Vol 4 (6) ◽

Cited By ~ 1

Author(s):

A. Mandal ◽

B. J. Jensen ◽

M. C. Hudspeth ◽

S. Root ◽

R. S. Crum ◽

...

Keyword(s):

Porous Solid ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Direct Observations

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Bulk modulus of H2O across the ice VII–ice X transition measured by time-resolved x-ray diffraction in dynamic diamond anvil cell experiments

Physical Review B ◽

10.1103/physrevb.103.064104 ◽

2021 ◽

Vol 103 (6) ◽

Author(s):

A. S. J. Méndez ◽

F. Trybel ◽

R. J. Husband ◽

G. Steinle-Neumann ◽

H.-P. Liermann ◽

...

Keyword(s):

Bulk Modulus ◽

Diamond Anvil Cell ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Diamond Anvil

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Spatially Resolved Forming Mechanisms Detection in Single Point Incremental Forming Using Synchrotron Based Texture Analysis

Metallurgical and Materials Transactions A ◽

10.1007/s11661-021-06261-1 ◽

2021 ◽

Author(s):

Mateus Dobecki ◽

Alexander Poeche ◽

Walter Reimers

Keyword(s):

Texture Analysis ◽

Incremental Forming ◽

Single Point ◽

High Energy ◽

X Ray Diffraction ◽

X Ray ◽

Forming Mechanism ◽

Spatially Resolved ◽

Step Down ◽

Stress States

AbstractDespite the ongoing success of understanding the deformation states in sheets manufactured by single-point incremental forming (SPIF), the unawareness of the spatially resolved influence of the forming mechanisms on the residual stress states of incrementally formed sheet metal parts impedes their application-optimized use. In this study, a well-founded experimental proof of the occurring forming mechanisms shear, bending and stretching is presented using spatially resolved, high-energy synchrotron x-ray diffraction-based texture analysis in transmission mode. The measuring method allows even near-surface areas to be examined without any impairment of microstructural influences due to tribological reactions. The depth-resolved texture evolution for different sets of forming parameters offers insights into the forming mechanisms acting in SPIF. Therefore, the forming mechanisms are triggered explicitly by adjusting the vertical step-down increment Δz for groove, plate and truncated cone geometries. The texture analysis reveals that the process parameters and the specimen geometries used lead to characteristic changes in the crystallites’ orientation distribution in the formed parts due to plastic deformation. These forming-induced reorientations of the crystallites could be assigned to the forming mechanisms by means of defined reference states. It was found that for groove, plate and truncated cone geometries, a decreasing magnitude of step-down increments leads to a more pronounced shear deformation, which causes an increasing work hardening especially at the tool contact area of the formed parts. Larger step-down increments, on the other hand, induce a greater bending deformation. The plastic deformation by bending leads to a complex stress field that involves alternating residual tensile stresses on the tool and residual compressive stresses on the tool-averted side incrementally formed sheets. The present study demonstrates the potential of high-energy synchrotron x-ray diffraction for the spatially resolved forming mechanism research in SPIF. Controlling the residual stress states by optimizing the process parameters necessitates knowledge of the fundamental forming mechanism action.

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Phase composition depth profiles using spatially resolved energy dispersive X-ray diffraction

Journal of Applied Crystallography ◽

10.1107/s0021889804024148 ◽

2004 ◽

Vol 37 (6) ◽

pp. 967-976 ◽

Cited By ~ 9

Author(s):

Andrew C. Jupe ◽

Stuart R. Stock ◽

Peter L. Lee ◽

Nikhila N. Naik ◽

Kimberly E. Kurtis ◽

...

Keyword(s):

Phase Composition ◽

Spatial Resolution ◽

Zinc Coating ◽

High Energy ◽

Sulfate Attack ◽

Energy Dispersive ◽

X Ray Diffraction ◽

X Ray ◽

Spatially Resolved ◽

Composition Profiles

Spatially resolved energy dispersive X-ray diffraction, using high-energy synchrotron radiation (∼35–80 keV), was used nondestructively to obtain phase composition profiles along the radii of cylindrical cement paste samples to characterize the progress of the chemical changes associated with sulfate attack on the cement. Phase distributions were acquired to depths of ∼4 mm below the specimen surface with sufficient spatial resolution to discern features less than 200 µm thick. The experimental and data analysis methods employed to obtain quantitative composition profiles are described. The spatial resolution that could be achieved is illustrated using data obtained from copper cylinders with a thin zinc coating. The measurements demonstrate that this approach is useful for nondestructively visualizing the sometimes complex transformations that take place during sulfate attack on cement-based materials. These transformations can be spatially related to microstructure as seen by computed microtomography.

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