<i>In Situ</i>Diffraction Measurements: Challenges, Instrumentation, and Examples

Ehrenberg, Helmut; Senyshyn, Anatoliy; Hinterstein, Manuel; Fueß, H.

doi:10.1002/9783527649884.ch16

Cited by 7 publications

(8 citation statements)

References 34 publications

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“…In such instance neutron scattering is already a well-established experimental technique for the characterization of complex Li-ion batteries. It has numerous advantages 2 : the high penetration depth of thermal neutrons permits non-destructive in situ and in operando studies of different kinds; the capability to localize light elements (e.g. hydrogen, lithium) and to resolve isotopes provides the necessary contrast; the neutron scattering length not dependent on momentum transfer, enabling to achieve accurate structure factors at high 2θ angles etc.…”

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confidence: 99%

Homogeneity of lithium distribution in cylinder-type Li-ion batteries

Senyshyn

Mühlbauer

Dolotko

et al. 2015

Sci Rep

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Spatially-resolved neutron powder diffraction with a gauge volume of 2 × 2 × 20 mm3 has been applied as an in situ method to probe the lithium concentration in the graphite anode of different Li-ion cells of 18650-type in charged state. Structural studies performed in combination with electrochemical measurements and X-ray computed tomography under real cell operating conditions unambiguously revealed non-homogeneity of the lithium distribution in the graphite anode. Deviations from a homogeneous behaviour have been found in both radial and axial directions of 18650-type cells and were discussed in the frame of cell geometry and electrical connection of electrodes, which might play a crucial role in the homogeneity of the lithium distribution in the active materials within each electrode.

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confidence: 99%

Homogeneity of lithium distribution in cylinder-type Li-ion batteries

Senyshyn

Mühlbauer

Dolotko

et al. 2015

Sci Rep

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“…However, sophisticated in situ or in operando experiments in materials science or for fundamental research, together with complex sample environments or transmission geometry setups, are frequently limited by absorption. Since the ideal ratio between absorption and sample thickness is reached at R = 1, with being the absorption coefficient and R being the sample radius, complex sample environments or geometries can only be realized with increasing photon energy and thus decreasing (Cullity & Stock, 2001;Ehrenberg et al, 2013Ehrenberg et al, , 2019. These experiments demand higher photon energies with a higher penetration depth or higher transmission capability (Schmitt et al, 2013;Ehrenberg et al, 2019).…”

Section: Introductionmentioning

confidence: 99%

“…Over recent decades the powder-diffraction technique has developed into one of the most powerful and versatile techniques for structural characterization of materials. It is routinely used in laboratory setups and also in synchrotron and neutron facilities, especially for in situ and in operando experiments (Ehrenberg et al, 2013(Ehrenberg et al, , 2019. During this development, sophisticated experiments progressively demanded the continuous increase of photon energy (Ehrenberg et al, 2013).…”

Section: Introductionmentioning

confidence: 99%

“…It is routinely used in laboratory setups and also in synchrotron and neutron facilities, especially for in situ and in operando experiments (Ehrenberg et al, 2013(Ehrenberg et al, , 2019. During this development, sophisticated experiments progressively demanded the continuous increase of photon energy (Ehrenberg et al, 2013). Conventional powder-diffraction beamlines usually operate at rather soft photon energies of up to 20-30 keV owing to the low critical energies of the source (Knapp et al, 2004;Patterson et al, 2005;Wallwork et al, 2007;Thompson et al, 2009;Yang et al, 2015;Lausi et al, 2015).…”

Section: Introductionmentioning

confidence: 99%

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Multi-analyser detector (MAD) for high-resolution and high-energy powder X-ray diffraction

et al. 2021

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For high-resolution powder diffraction in material science, high photon energies are necessary, especially for in situ and in operando experiments. For this purpose, a multi-analyser detector (MAD) was developed for the high-energy beamline P02.1 at PETRA III of the Deutsches Elektronen-Synchrotron (DESY). In order to be able to adjust the detector for the high photon energies of 60 keV, an individually adjustable analyser–crystal setup was designed. The adjustment is performed via piezo stepper motors for each of the ten channels. The detector shows a low and flat background as well as a high signal-to-noise ratio. A range of standard materials were measured for characterizing the performance. Two exemplary experiments were performed to demonstrate the potential for sophisticated structural analysis with the MAD: (i) the structure of a complex material based on strontium niobate titanate and strontium niobate zirconate was determined and (ii) an in situ stroboscopy experiment with an applied electric field on a highly absorbing piezoceramic was performed. These experiments demonstrate the capabilities of the new MAD, which advances the frontiers of the structural characterization of materials.

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“…For example, in situ hydrogenation measurements on materials suitable for concentrated solar power (Sheppard et al, 2014;Humphries et al, 2016) 2017; Dolci et al, 2010;Frommen et al, 2015) could help researchers to understand reaction pathways. Furthermore, operando multi-parameter studies could be undertaken to follow structural changes in magnetic and electrical fields (Ehrenberg et al, 2012;Gilmore et al, 2018) or in ferroelectric materials (Hinterstein et al, 2015), or to carry out simultaneous electrochemical and powder diffraction measurements on batteries (Senyshyn et al, 2013). With the second detector, spatially resolved diffraction studies can be carried out, e.g.…”

Section: Introductionmentioning

confidence: 99%