Journal articles: 'TIME-RESOLVED ION IMAGING'

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Fisher-Levine, Merlin, Rebecca Boll, Farzaneh Ziaee, Cédric Bomme, Benjamin Erk, Dimitrios Rompotis, Tatiana Marchenko, Andrei Nomerotski, and Daniel Rolles. "Time-resolved ion imaging at free-electron lasers using TimepixCam." Journal of Synchrotron Radiation 25, no. 2 (February 20, 2018): 336–45. http://dx.doi.org/10.1107/s1600577517018306.

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The application of a novel fast optical-imaging camera, TimepixCam, to molecular photoionization experiments using the velocity-map imaging technique at a free-electron laser is described. TimepixCam is a 256 × 256 pixel CMOS camera that is able to detect and time-stamp ion hits with 20 ns timing resolution, thus making it possible to record ion momentum images for all fragment ions simultaneously and avoiding the need to gate the detector on a single fragment. This allows the recording of significantly more data within a given amount of beam time and is particularly useful for pump–probe experiments, where drifts, for example, in the timing and pulse energy of the free-electron laser, severely limit the comparability of pump–probe scans for different fragments taken consecutively. In principle, this also allows ion–ion covariance or coincidence techniques to be applied to determine angular correlations between fragments.

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Wells, Kym L., Gareth Perriam, and Vasilios G. Stavros. "Time-resolved velocity map ion imaging study of NH3 photodissociation." Journal of Chemical Physics 130, no. 7 (February 21, 2009): 074308. http://dx.doi.org/10.1063/1.3072763.

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Wang, Qin-xin, Dan-dan Shi, Jun-feng Zhang, Xue Wang, Yu Si, Chun-bin Gao, Jian Fang, and Si-zuo Luo. "Channel-resolved ultrafast dissociation dynamics of NO2 molecules studied via femtosecond time-resolved ion imaging." Chinese Journal of Chemical Physics 32, no. 3 (June 2019): 292–98. http://dx.doi.org/10.1063/1674-0068/cjcp1807177.

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Ruedas-Rama, Maria J., Angel Orte, Elizabeth A. H. Hall, Jose M. Alvarez-Pez, and Eva M. Talavera. "A chloride ion nanosensor for time-resolved fluorimetry and fluorescence lifetime imaging." Analyst 137, no. 6 (2012): 1500. http://dx.doi.org/10.1039/c2an15851e.

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Toulson, Benjamin W., Dmitry A. Fishman, and Craig Murray. "Photodissociation dynamics of acetone studied by time-resolved ion imaging and photofragment excitation spectroscopy." Physical Chemistry Chemical Physics 20, no. 4 (2018): 2457–69. http://dx.doi.org/10.1039/c7cp07320h.

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The photodissociation dynamics of acetone has been investigated using velocity-map ion imaging and photofragment excitation (PHOFEX) spectroscopy across a range of wavelengths spanning the first absorption band (236–308 nm).

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Malakar, Y., W. L. Pearson, M. Zohrabi, B. Kaderiya, Kanaka Raju P., F. Ziaee, S. Xue, et al. "Time-resolved imaging of bound and dissociating nuclear wave packets in strong-field ionized iodomethane." Physical Chemistry Chemical Physics 21, no. 26 (2019): 14090–102. http://dx.doi.org/10.1039/c8cp07032f.

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We report the results of a time-resolved coincident ion momentum imaging experiment probing nuclear wave packet dynamics in the strong-field ionization and dissociation of iodomethane (CH₃I).

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Bufford, Daniel, Sarah H. Pratt, Timothy J. Boyle, and Khalid Hattar. "Time-Resolved 3D Imaging of Ion Beam Induced Surface Damage in Gold Nanoparticles." Microscopy and Microanalysis 20, S3 (August 2014): 800–801. http://dx.doi.org/10.1017/s1431927614005728.

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Laird, Jamie S., Brett C. Johnson, Kumaravelu Ganesan, Sasikaran Kandasamy, Garry Davidson, Stacey Borg, and Chris G. Ryan. "Impurity mapping in sulphide minerals using Time-resolved Ion Beam Induced Current imaging." Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 268, no. 11-12 (June 2010): 1903–10. http://dx.doi.org/10.1016/j.nimb.2010.02.095.

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Toulson, Benjamin W., Kara M. Kapnas, Dmitry A. Fishman, and Craig Murray. "Competing pathways in the near-UV photochemistry of acetaldehyde." Physical Chemistry Chemical Physics 19, no. 22 (2017): 14276–88. http://dx.doi.org/10.1039/c7cp02573d.

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Harrison, Jeffrey S., Dean A. Waldow, Phillip A. Cox, Rajiv Giridharagopal, Marisa Adams, Victoria Richmond, Sevryn Modahl, Megan Longstaff, Rodion Zhuravlev, and David S. Ginger. "Noncontact Imaging of Ion Dynamics in Polymer Electrolytes with Time-Resolved Electrostatic Force Microscopy." ACS Nano 13, no. 1 (December 19, 2018): 536–43. http://dx.doi.org/10.1021/acsnano.8b07254.

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Slaughter, D. S., K. A. Larsen, F. P. Sturm, A. Belkacem, P. Ranitovic, and Th Weber. "Ultrafast time-resolved photoelectron and ion fragment momentum imaging of vacuum ultraviolet-excited molecules." Journal of Physics: Conference Series 1412 (January 2020): 072048. http://dx.doi.org/10.1088/1742-6596/1412/7/072048.

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Stewart, Ian I., Carl E. Hensman, and John W. Olesik. "Influence of Gas Sampling on Analyte Transport within the ICP and Ion Sampling for ICP-MS Studied Using Individual, Isolated Sample Droplets." Applied Spectroscopy 54, no. 2 (February 2000): 164–74. http://dx.doi.org/10.1366/0003702001949230.

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The effect of gas flow entrainment on the gas sampling, ion sampling, and ion detection processes in inductively coupled plasma mass spectrometry (ICP-MS) has been investigated. Isolated, single droplets of sample from a monodisperse dried microparticulate injector (MDMI) were used in conjunction with time-resolved ICP-MS, photographs of ion cloud movement, and time-gated imaging using a gateable, intensified charge-coupled device (ICCD) detector mounted on an imaging spectrometer. The results indicate that gas flow entrainment into the sampling orifice can have a significant effect on the plasma gas velocities as far as 7 mm from the sampling orifice. The effects are most pronounced within 3 mm of the sampling orifice. The trends in these results are consistent with theoretical calculations. Photographic images show that plasma gas initially as far as 3 mm off axis adopts a curved path into the sampling orifice. Time-resolved emission images of Sr+ ion clouds approaching the sampling orifice demonstrate the entrainment process and significant distortion of the ion cloud as it flows into the sampling orifice. Spatial maps of La+ ICP-MS signals were acquired as a function of distance from the vaporization point and distance from the plasma axis. The results suggest that gas entrainment has a significant effect on the spatial path of ions in the plasma and that accurate radially resolved spatial mapping of plasmas using mass spectrometry may not be possible. The widths of radially resolved La+ ICP-MS signal peaks do not change significantly when ions are sampled 2 mm from the vaporization point compared to 5 mm away. In contrast, ICP-MS signals measured on axis as a function of time clearly show broadening due to diffusion. These observations suggest that some detected ions may have originated from off-axis locations in the plasma.

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Bull, James N., Christopher W. West, Cate S. Anstöter, Gabriel da Silva, Evan J. Bieske, and Jan R. R. Verlet. "Ultrafast photoisomerisation of an isolated retinoid." Physical Chemistry Chemical Physics 21, no. 20 (2019): 10567–79. http://dx.doi.org/10.1039/c9cp01624d.

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The photoinduced excited state dynamics of gas-phase trans-retinoate (deprotonated trans-retinoic acid, trans-RA⁻) are studied using tandem ion mobility spectrometry coupled with laser spectroscopy, and frequency-, angle- and time-resolved photoelectron imaging.

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Forbes, Ruaridh, Varun Makhija, Kévin Veyrinas, Albert Stolow, Jason W. L. Lee, Michael Burt, Mark Brouard, et al. "Time-resolved multi-mass ion imaging: Femtosecond UV-VUV pump-probe spectroscopy with the PImMS camera." Journal of Chemical Physics 147, no. 1 (July 7, 2017): 013911. http://dx.doi.org/10.1063/1.4978923.

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Liu, Shujuan, Aqiang Xu, Zejing Chen, Yun Ma, Huiran Yang, Zhengjian Shi, and Qiang Zhao. "Phosphorescent ion-paired iridium(III) complex for ratiometric and time-resolved luminescence imaging of intracellular biothiols." Optics Express 24, no. 25 (November 28, 2016): 28247. http://dx.doi.org/10.1364/oe.24.028247.

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Yukihara, Eduardo G., Brandon A. Doull, Md Ahmed, Stephan Brons, Thomas Tessonnier, Oliver Jäkel, and Steffen Greilich. "Time-resolved optically stimulated luminescence of Al2O3:C for ion beam therapy dosimetry." Physics in Medicine and Biology 60, no. 17 (August 13, 2015): 6613–38. http://dx.doi.org/10.1088/0031-9155/60/17/6613.

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Datta, R., D. R. Russell, I. Tang, T. Clayson, L. G. Suttle, J. P. Chittenden, S. V. Lebedev, and J. D. Hare. "Time-resolved velocity and ion sound speed measurements from simultaneous bow shock imaging and inductive probe measurements." Review of Scientific Instruments 93, no. 10 (October 1, 2022): 103530. http://dx.doi.org/10.1063/5.0098823.

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We present a technique to measure the time-resolved velocity and ion sound speed in magnetized, supersonic high-energy-density plasmas. We place an inductive (“b-dot”) probe in a supersonic pulsed-power-driven plasma flow and measure the magnetic field advected by the plasma. As the magnetic Reynolds number is large ( R M > 10), the plasma flow advects a magnetic field proportional to the current at the load. This enables us to estimate the flow velocity as a function of time from the delay between the current at the load and the signal at the probe. The supersonic flow also generates a hydrodynamic bow shock around the probe, the structure of which depends on the upstream sonic Mach number. By imaging the shock around the probe with a Mach–Zehnder interferometer, we determine the upstream Mach number from the shock Mach angle, which we then use to determine the ion sound speed from the known upstream velocity. We use the sound speed to infer the value of [Formula: see text], where [Formula: see text] is the average ionization and T e is the electron temperature. We use this diagnostic to measure the time-resolved velocity and sound speed of a supersonic ( M S ∼ 8), super-Alfvénic ( M A ∼ 2) aluminum plasma generated during the ablation stage of an exploding wire array on the Magpie generator (1.4 MA, 250 ns). The velocity and [Formula: see text] measurements agree well with the optical Thompson scattering measurements reported in the literature and with 3D resistive magnetohydrodynamic simulations in GORGON.

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Boll, Rebecca, Arnaud Rouzée, Marcus Adolph, Denis Anielski, Andrew Aquila, Sadia Bari, Cédric Bomme, et al. "Imaging molecular structure through femtosecond photoelectron diffraction on aligned and oriented gas-phase molecules." Faraday Discuss. 171 (2014): 57–80. http://dx.doi.org/10.1039/c4fd00037d.

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This paper gives an account of our progress towards performing femtosecond time-resolved photoelectron diffraction on gas-phase molecules in a pump–probe setup combining optical lasers and an X-ray free-electron laser. We present results of two experiments aimed at measuring photoelectron angular distributions of laser-aligned 1-ethynyl-4-fluorobenzene (C₈H₅F) and dissociating, laser-aligned 1,4-dibromobenzene (C₆H₄Br₂) molecules and discuss them in the larger context of photoelectron diffraction on gas-phase molecules. We also show how the strong nanosecond laser pulse used for adiabatically laser-aligning the molecules influences the measured electron and ion spectra and angular distributions, and discuss how this may affect the outcome of future time-resolved photoelectron diffraction experiments.

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He, Zhi-gang, Zhi-chao Chen, Dong-yuan Yang, Dong-xu Dai, Guo-rong Wu, and Xue-ming Yang. "A New kHz Velocity Map Ion/Electron Imaging Spectrometer for Femtosecond Time-Resolved Molecular Reaction Dynamics Studies." Chinese Journal of Chemical Physics 30, no. 3 (June 27, 2017): 247–52. http://dx.doi.org/10.1063/1674-0068/30/cjcp1702018.

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20

Ellis, Shane R., Jens Soltwisch, and Ron M. A. Heeren. "Time-Resolved Imaging of the MALDI Linear-TOF Ion Cloud: Direct Visualization and Exploitation of Ion Optical Phenomena Using a Position- and Time-Sensitive Detector." Journal of The American Society for Mass Spectrometry 25, no. 5 (March 22, 2014): 809–19. http://dx.doi.org/10.1007/s13361-014-0839-6.

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HIRSCH, J. S., K. D. KAVANAGH, E. T. KENNEDY, J. T. COSTELLO, P. NICOLOSI, and L. POLETTO. "Tracking ground state Ba+ions in an expanding laser–plasma plume using time-resolved vacuum ultraviolet photoionization imaging." Laser and Particle Beams 22, no. 3 (July 2004): 207–13. http://dx.doi.org/10.1017/s0263034604223035.

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We report results from a study of the integrated column density and expansion dynamics of ground-state-selected Ba+ions in a laser–plasma plume using a new experimental system—VPIF (vacuum-ultraviolet photoabsorption imaging facility). The ions are tracked by recording the attenuation of a pulsed and collimated vacuum ultraviolet beam, tuned to the 5p–6dinner-shell resonance of singly ionized barium, as the expanding plasma plume moves across it. The attenuated beam is allowed to fall on a CCD array where the spatial distribution of the absorption is recorded. Time-resolved ion velocity and integrated column density maps are readily extracted from the photoionization images.

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Yuan, Kai-Jun, and André D. Bandrauk. "Probing Attosecond Electron Coherence in Molecular Charge Migration by Ultrafast X-Ray Photoelectron Imaging." Applied Sciences 9, no. 9 (May 11, 2019): 1941. http://dx.doi.org/10.3390/app9091941.

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Electron coherence is a fundamental quantum phenomenon in today’s ultrafast physics and chemistry research. Based on attosecond pump–probe schemes, ultrafast X-ray photoelectron imaging of molecules was used to monitor the coherent electron dynamics which is created by an XUV pulse. We performed simulations on the molecular ion H 2 + by numerically solving time-dependent Schrödinger equations. It was found that the X-ray photoelectron angular and momentum distributions depend on the time delay between the XUV pump and soft X-ray probe pulses. Varying the polarization and helicity of the soft X-ray probe pulse gave rise to a modulation of the time-resolved photoelectron distributions. The present results provide a new approach for exploring ultrafast coherent electron dynamics and charge migration in reactions of molecules on the attosecond time scale.

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Souto, Ricardo M., Dániel Filotás, Bibiana M. Fernández-Pérez, Lívia Nagy, and Géza Nagy. "New Developments in Scanning Microelectrochemical Techniques: A Highly Sensitive Route to Evaluate Degradation Reactions and Protection Methods with Chemical Selectivity." Applied Mechanics and Materials 875 (January 2018): 19–23. http://dx.doi.org/10.4028/www.scientific.net/amm.875.19.

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The scanning electrochemical microscope (SECM) offers a highly sensitive route to evaluate degradation reactions and protection methods with chemical selectivity by using ion-selective microelectrodes as tips, thus operating SECM potentiometrically. Spatially resolved imaging of electrochemical reactivity related to each component of the investigated material can thus be effectively monitored selectively both in situ and in real time. The applicability of this method has been illustrated using a practical example of a metal-coating system, consisting in the exposure of cut edges of coil-coated galvanized steel to aqueous saline environment. In this contribution, localized pH and zinc(II) ion distributions originated around cut edges of coil coated steel immersed in 1 mM NaCl solution are shown.

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Zhang, Ye, Dylan Lu, Mengyu Gao, Minliang Lai, Jia Lin, Teng Lei, Zhenni Lin, Li Na Quan, and Peidong Yang. "Quantitative imaging of anion exchange kinetics in halide perovskites." Proceedings of the National Academy of Sciences 116, no. 26 (June 12, 2019): 12648–53. http://dx.doi.org/10.1073/pnas.1903448116.

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Ion exchange, as a postsynthetic transformation strategy, offers more flexibilities in controlling material compositions and structures beyond direct synthetic methodology. Observation of such transformation kinetics on the single-particle level with rich spatial and spectroscopic information has never been achieved. We report the quantitative imaging of anion exchange kinetics in individual single-crystalline halide perovskite nanoplates using confocal photoluminescence microscopy. We have systematically observed a symmetrical anion exchange pathway on the nanoplates with dependence on reaction time and plate thickness, which is governed by the crystal structure and the diffusion-limited transformation mechanism. Based on a reaction–diffusion model, the halide diffusion coefficient was estimated to be on the order of10−14cm2⋅s−1. This diffusion-controlled mechanism leads to the formation of 2D perovskite heterostructures with spatially resolved coherent interface through the precisely controlled anion exchange reaction, offering a design protocol for tailoring functionalities of semiconductors at the nano-/microscale.

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Finšgar, Matjaž. "2-Phenylimidazole Corrosion Inhibitor on Copper: An XPS and ToF-SIMS Surface Analytical Study." Coatings 11, no. 8 (August 13, 2021): 966. http://dx.doi.org/10.3390/coatings11080966.

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This work presents a surface analytical study of the corrosion inhibitor 2-phenylimidazole (2PhI) adsorbed on a Cu surface from 3 wt.% NaCl solution. X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were used to investigate the surface phenomena. Various XPS experiments were performed, i.e., survey- and angle-resolved high-resolution XPS spectra measurements, gas cluster ion beam sputtering in conjunction with XPS measurements, and XPS imaging in conjunction with principal component analysis. These measurements were used to detail the composition of the surface layer at depth. In addition, various ToF-SIMS experiments were performed, such as positive ion ToF-SIMS spectral measurements, ToF-SIMS imaging, and cooling/heating in conjunction with ToF-SIMS measurements. This study shows that organometallic complexes were formed between 2PhI molecules and Cu ions, that the surface layer contained entrapped NaCl, that the surface layer contained some Cu(II) species (but the majority of species were Cu(I)-containing species), that the surface was almost completely covered with a combination of 2PhI molecules and organometallic complex, and that the temperature stability of these species increases when 2PhI is included in the organometallic complex.

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Naselli, Eugenia, Richard Rácz, Sandor Biri, Maria Mazzaglia, Luigi Celona, Santo Gammino, Giuseppe Torrisi, Zoltan Perduk, Alessio Galatà, and David Mascali. "Innovative Analytical Method for X-ray Imaging and Space-Resolved Spectroscopy of ECR Plasmas." Condensed Matter 7, no. 1 (December 28, 2021): 5. http://dx.doi.org/10.3390/condmat7010005.

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At the Italian National Institute for Nuclear Physics-Southern National Laboratory (INFN-LNS), and in collaboration with the ATOMKI laboratories, an innovative multi-diagnostic system with advanced analytical methods has been designed and implemented. This is based on several detectors and techniques (Optical Emission Spectroscopy, RF systems, interfero-polarimetry, X-ray detectors), and here we focus on high-resolution, spatially resolved X-ray spectroscopy, performed by means of a X-ray pin-hole camera setup operating in the 0.5–20 keV energy domain. The diagnostic system was installed at a 14 GHz Electron Cyclotron Resonance (ECR) ion source (ATOMKI, Debrecen), enabling high-precision, X-ray, spectrally resolved imaging of ECR plasmas heated by hundreds of Watts. The achieved spatial and energy resolutions were 0.5 mm and 300 eV at 8 keV, respectively. Here, we present the innovative analysis algorithm that we properly developed to obtain Single Photon-Counted (SPhC) images providing the local plasma-emitted spectrum in a High-Dynamic-Range (HDR) mode, by distinguishing fluorescence lines of the materials of the plasma chamber (Ti, Ta) from plasma (Ar). This method allows for a quantitative characterization of warm electrons population in the plasma (and its 2D distribution), which are the most important for ionization, and to estimate local plasma density and spectral temperatures. The developed post-processing analysis is also able to remove the readout noise that is often observable at very low exposure times (msec). The setup is now being updated, including fast shutters and trigger systems to allow simultaneous space and time-resolved plasma spectroscopy during transients, stable and turbulent regimes.

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Rodrigues, N. D. N., M. Staniforth, J. D. Young, Y. Peperstraete, N. C. Cole-Filipiak, J. R. Gord, P. S. Walsh, D. M. Hewett, T. S. Zwier, and V. G. Stavros. "Towards elucidating the photochemistry of the sunscreen filter ethyl ferulate using time-resolved gas-phase spectroscopy." Faraday Discussions 194 (2016): 709–29. http://dx.doi.org/10.1039/c6fd00079g.

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Ultrafast time-resolved ion yield (TR-IY) and velocity map imaging spectroscopies are employed to reveal the relaxation dynamics after photoexcitation in ethyl 4-hydroxy-3-methoxycinnamate (ethyl ferulate, EF), an active ingredient in commercially available sunscreens. In keeping with a bottom-up strategy, the building blocks of EF, 2-methoxy-4-vinylphenol (MVP) and 4-hydroxy-3-methoxycinnamyl alcohol (coniferyl alcohol, ConA), were also studied to assist in our understanding of the dynamics of EF as we build up in molecular complexity. In contrast to the excited state dynamics of MVP and ConA, which are described by a single time constant (>900 ps), the dynamics of EF are described by three time constants (15 ± 4 ps, 148 ± 47 ps, and >900 ps). A mechanism is proposed involving internal conversion (IC) between the initially excited S₁(1¹ππ*) and S₂(1¹nπ*) states followed by intramolecular vibrational redistribution (IVR) on both states, in competition with intersystem crossing onto neighbouring triplet states (15 ± 4 ps). IVR and IC within the triplet manifold then ensues (148 ± 47 ps) to populate a low-lying triplet state (>900 ps). Importantly, the fluorescence spectrum of EF at the S₁origin, along with the associated lifetime (6.9 ± 0.1 ns), suggests that population is trapped, during initial IVR, on the S₁(1¹ππ*) state. This serves to demonstrate the complex, competing dynamics in this sunscreen filter molecule.

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Suchorski, Y., J. Zeininger, S. Buhr, M. Raab, M. Stöger-Pollach, J. Bernardi, H. Grönbeck, and G. Rupprechter. "Resolving multifrequential oscillations and nanoscale interfacet communication in single-particle catalysis." Science 372, no. 6548 (May 20, 2021): 1314–18. http://dx.doi.org/10.1126/science.abf8107.

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In heterogeneous catalysis research, the reactivity of individual nanofacets of single particles is typically not resolved. We applied in situ field electron microscopy to the apex of a curved rhodium crystal (radius of 650 nanometers), providing high spatial (~2 nanometers) and time resolution (~2 milliseconds) of oscillatory catalytic hydrogen oxidation, to image adsorbed species and reaction fronts on the individual facets. Using ionized water as the imaging species, the active sites were directly imaged with field ion microscopy. The catalytic behavior of differently structured nanofacets and the extent of coupling between them were monitored individually. We observed limited interfacet coupling, entrainment, frequency locking, and reconstruction-induced collapse of spatial coupling. The experimental results are backed up by microkinetic modeling of time-dependent oxygen species coverages and oscillation frequencies.

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Ziesche, Ralf F., Anton S. Tremsin, Chun Huang, Chun Tan, Patrick S. Grant, Malte Storm, Dan J. L. Brett, Paul R. Shearing, and Winfried Kockelmann. "4D Bragg Edge Tomography of Directional Ice Templated Graphite Electrodes." Journal of Imaging 6, no. 12 (December 11, 2020): 136. http://dx.doi.org/10.3390/jimaging6120136.

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Bragg edge tomography was carried out on novel, ultra-thick, directional ice templated graphite electrodes for Li-ion battery cells to visualise the distribution of graphite and stable lithiation phases, namely LiC12 and LiC6. The four-dimensional Bragg edge, wavelength-resolved neutron tomography technique allowed the investigation of the crystallographic lithiation states and comparison with the electrode state of charge. The tomographic imaging technique provided insight into the crystallographic changes during de-/lithiation over the electrode thickness by mapping the attenuation curves and Bragg edge parameters with a spatial resolution of approximately 300 µm. This feasibility study was performed on the IMAT beamline at the ISIS pulsed neutron spallation source, UK, and was the first time the 4D Bragg edge tomography method was applied to Li-ion battery electrodes. The utility of the technique was further enhanced by correlation with corresponding X-ray tomography data obtained at the Diamond Light Source, UK.

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Hofmann, Felix, Nicholas W. Phillips, Ross J. Harder, Wenjun Liu, Jesse N. Clark, Ian K. Robinson, and Brian Abbey. "Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements." Journal of Synchrotron Radiation 24, no. 5 (August 8, 2017): 1048–55. http://dx.doi.org/10.1107/s1600577517009183.

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Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focused ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.

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Fried, Daniel, Gene P. Reck, Toshimoto Kushida, Gyung-Soo Kim, and Erhard W. Rothe. "Imaging of the Fluorescence Created by Ablation of Y2O3, BaO2, CuO, and YBa2Cu3O7–x by 308-nm Laser Light." Applied Spectroscopy 47, no. 7 (July 1993): 1046–57. http://dx.doi.org/10.1366/0003702934415426.

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A gated intensified CCD camera is used to acquire time-resolved images of the plume generated from the excimer laser ablation of CuO, BaO2, Y2O3, and YBa2Cu3O7– x pellets in vacuum, He, or O2. Narrow (12-nm FWHM) bandpass filters are used to select emission from individual species within the plume. The spatial and the temporal evolution of the emission is unique for each of the ejected ions, atoms, and diatomics. A luminous shock front, i.e., a blast wave, is observed at pressures greater than 1 Torr in He and 0.1 Torr in O2. The propagation of this shock front is suitably described by scaling factors that were previously developed to describe the shock waves from a point explosion. Images of emission from atomic Cu and O were acquired after the ablation of CuO. These images imply that ion/electron bombardment is significant within the plasma plume. The time dependence of the images shows the evolution of the shock wave and suggests the origin of the luminous plume.

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Cox, Dalton, and Scott A. Barnett. "Time-Resolved Characterization of Electrochemically-Induced Solid Oxide Cell Microstructure Evolution." ECS Meeting Abstracts MA2022-01, no. 37 (July 7, 2022): 1620. http://dx.doi.org/10.1149/ma2022-01371620mtgabs.

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Solid oxide cells (SOC) are exciting both for their capability of fuel-flexible electricity generation and their promise in the production of green H2; however, their degradation and long-term performance remain important questions. Operating individual button cells to characterize these changes is prone to cell-to-cell variations, whereas large-area cell/stack life testing requires considerable resources. In both cases, full cell characterization usually must wait until the completion of the life test, which may delay getting results for months or years. While progress has been made in observing microstructural changes over time (termed here time-resolved characterization) using techniques like non-destructive transmission x-ray microscope tomography, such experiments are difficult to implement, especially the effect of current is unexplored due to geometrical and gas environmental limitations of the system. Presented here is a method to rapidly obtain time-resolved microstructural information of the same cell in tandem with electrochemical measurements. While SOC degradation arises due to a range of processes, this work focuses on the microstructural evolution of Ni-YSZ fuel electrodes that occurs during electrolysis operation, which is known to be a key issue. Two key experimental features allowed time-resolved characterization of multiple cells simultaneously: (1) the use of Ni-YSZ symmetric cells allows multiple cells of different size in a single test by avoiding the need for gas seals, and (2) the use of laser milling to allow controlled removal of a portion of each cell during the test. Here we illustrate the method for the case of low steam content and high current density, designed to exacerbate and accelerate electrolysis degradation due to the highly reducing conditions achieved. Tape-cast planar electrode-supported Ni-YSZ symmetric cells were laser cut into precise geometries with well-defined projected areas and easily removable sections. Four cells with projected areas of 1, 1, 0.75, and 0.5 cm2 were connected in series within the same furnace at 800 C and a gas environment of 97% H2 and 3% H2O. A current of 0.75 A was run through three of the cells, resulting in current densities of 0.75, 1.0, and 1.5 A/cm2, while one was maintained with no current. The life test lasted for 500 h, and the microstructure was observed at 0, 200, and 500 hours. Figure 1 shows the microstructures observed at the highest current density by polished cross-sectional SEM and FIB-polished sections under conditions that provided Ni/YSZ contrast. Microstructural degradation had occurred by 200 h and became immense at 500 h, due to high current density in these reducing conditions. By 200 hours, grain boundaries become enriched with Ni, likely due to the formation of Ni-Zr intermetallics in the ultra-low pO2 induced by local overpotential as reported by Chen[1] and Szasz[2]. Additionally, the electrode-electrolyte interface becomes nanoporous and a Ni enriched fracture is present ~2 μm into the electrolyte. By 500 hours, the Ni rich nanoporosity has progressed more than 10 μm into the electrolyte and created islands of large grains surrounded by Ni-rich deposits. Electrochemical impedance spectroscopy measurements show a clear initial decrease in polarization resistance followed by an overall impedance increase by 200 hours. These correspond to the initial electrochemical boost from the production of a nanoporous structure, followed by the deactivation of areas of the cell due to the large fractures through the electrolyte. [1] M. Chen et al., “Microstructural Degradation of Ni/YSZ Electrodes in Solid Oxide Electrolysis Cells under High Current,” J. Electrochem. Soc., vol. 160, no. 8, pp. F883–F891, 2013, doi: 10.1149/2.098308jes. [2] J. Szász et al., “High-Resolution Studies on Nanoscaled Ni/YSZ Anodes,” Chem. Mater., vol. 29, no. 12, pp. 5113–5123, 2017, doi: 10.1021/acs.chemmater.7b00360. Figure 1: Microstructural and electrochemical changes of a symmetric Ni-YSZ SOC undergoing 1.5 A/cm2 in reducing conditions at 0, 200, and 500 hours. Cathode is on the left in all images; anode is on the right. a, b, c) Backscatter electron imaging reveals destruction of the dense YSZ electrolyte over the lifetime of the experiment. Lines of brighter phases on the anode side of fractures are Ni deposits. d, e, f) Focused Ion Beam cross sections reveal nanoporosity forming in the first 10 μm from the cathode-electrolyte interface at 200 and 500 hours. Charging is evident as a result of curtaining from the nanoporous features in the electrolyte. g) Electrochemical impedance spectroscopy shows the initial decrease in resistance from 0 to 48 hours followed by increasing resistance due to microstructure evolution. Figure 1

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Lowndes, D. H., S. J. Pennycook, G. E. Jellison, S. P. Withrow, and D. N. Mashburn. "Solidification of highly undercooled liquid silicon produced by pulsed laser melting of ion-implanted amorphous silicon: Time-resolved and microstructural studies." Journal of Materials Research 2, no. 5 (October 1987): 648–80. http://dx.doi.org/10.1557/jmr.1987.0648.

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Nanosecond resolution time-resolved visible (632.8 nm) and infrared (1152 nm) reflectivity measurements, together with structural and Z-contrast transmission electron microscope (TEM) imaging, have been used to study pulsed laser melting and subsequent solidification of thick (190–410 nm) amorphous (a) Si layers produced by ion implantation. Melting was initiated using a KrF (248 nm) excimer laser of relatively long [45 ns full width half maximum (FWHM)] pulse duration; the microstructural and time-resolved measurements cover the entire energy density (E1) range from the onset of melting (at ∼ 0.12J/cm2) up to the onset of epitaxial regrowth (at ∼ 1.1 J/cm2). At low E1 the infrared reflectivity measurements were used to determine the time of formation, the velocity, and the final depth of “explosively” propagating buried liquid layers in 410 nm thick a-Si specimens that had been uniformly implanted with Si, Ge, or Cu over their upper ∼ 300 nm. Measured velocities lie in the 8–14 m/s range, with generally higher velocities obtained for the Ge- and Cu-implanted “a-Si alloys.” The velocity measurements result in an upper limit of 17 (± 3) K on the undercooling versus velocity relationship for an undercooled solidfying liquid-crystalline Si interface. The Z-contrast scanning TEM measurements of the final buried layer depth were in excellent agreement with the optical measurements. The TEM study also shows that the “fine-grained polycrystalline Si” region produced by explosive crystallization of a-Si actually contains large numbers of disk-shaped Si flakes that can be seen only in plan view. These Si flakes have highly amorphous centers and laterally increasing crystallinity; they apparently grow primarily in the lateral direction. Flakes having this structure were found both at the surface, at low laser E1, and also deep beneath the surface, throughout the “fine-grained poly-Si” region formed by explosive crystallization, at higher E1. Our conclusion that this region is partially amorphous (the centers of flakes) differs from earlier results. The combined structural and optical measurements suggest that Si flakes nucleate at the undercooled liquid-amorphous interface and are the crystallization events that initiate explosive crystallization. Time-resolved reflectivity measurements reveal that the surface melt duration of the 410 nm thick a-Si specimens increases rapidly for 0.3E1 <0.6 J/cm2, but then remains nearly constant for E1 up to ∼ 1.0 J/cm2. For 0.3 < E1 < 0.6 J/cm2 the reflectivity exhibits a slowly decaying behavior as the near-surface pool of liquid Si fills up with growing large grains of Si. For higher E1, a flat-topped reflectivity signal is obtained and the microstructural and optical studies together show that the principal process occurring is increasingly deep melting followed by more uniform regrowth of large grains back to the surface. However, cross-section TEM shows that a thin layer of fine-grained poly-Si still is formed deep beneath the surface for E1<0.9 J/cm2, implying that explosive crystallization occurs (probably early in the laser pulse) even at these high E1 values. The onset of epitaxial regrowth at E1 = 1.1 J/cm2 is marked by a slight decrease in surface melt duration.

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Sjövall, Peter, Sebastien Gregoire, William Wargniez, Lisa Skedung, and Gustavo S. Luengo. "3D Molecular Imaging of Stratum Corneum by Mass Spectrometry Suggests Distinct Distribution of Cholesteryl Esters Compared to Other Skin Lipids." International Journal of Molecular Sciences 23, no. 22 (November 9, 2022): 13799. http://dx.doi.org/10.3390/ijms232213799.

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The crucial barrier properties of the stratum corneum (SC) depend critically on the design and integrity of its layered molecular structure. However, analysis methods capable of spatially resolved molecular characterization of the SC are scarce and fraught with severe limitations, e.g., regarding molecular specificity or spatial resolution. Here, we used 3D time-of-flight secondary ion mass spectrometry to characterize the spatial distribution of skin lipids in corneocyte multilayer squams obtained by tape stripping. Depth profiles of specific skin lipids display an oscillatory behavior that is consistent with successive monitoring of individual lipid and corneocyte layers of the SC structure. Whereas the most common skin lipids, i.e., ceramides, C24:0 and C26:0 fatty acids and cholesteryl sulfate, are similarly organized, a distinct 3D distribution was observed for cholesteryl oleate, suggesting a different localization of cholesteryl esters compared to the lipid matrix separating the corneocyte layers. The possibility to monitor the composition and spatial distribution of endogenous lipids as well as active drug and cosmetic substances in individual lipid and corneocyte layers has the potential to provide important contributions to the basic understanding of barrier function and penetration in the SC.

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Zhong, Xin, Xinwei Wang, Liang Sun, and Yan Zhou. "Enhancement of rapid lifetime determination for time-resolved fluorescence imaging in forensic examination." Chinese Optics Letters 19, no. 4 (2021): 041101. http://dx.doi.org/10.3788/col202119.041101.

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Zhong, Xin, Xinwei Wang, Liang Sun, and Yan Zhou. "Enhancement of rapid lifetime determination for time-resolved fluorescence imaging in forensic examination." Chinese Optics Letters 19, no. 4 (2021): 041101. http://dx.doi.org/10.3788/col202119.041101.

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Finšgar, Matjaž. "The Interface Characterization of 2-Mercapto-1-methylimidazole Corrosion Inhibitor on Brass." Coatings 11, no. 3 (March 4, 2021): 295. http://dx.doi.org/10.3390/coatings11030295.

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This work presents a detailed surface analytical study and surface characterization, with an emphasis on the X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) analyses of 2‑mercapto‑1‑methylimidazole (MMI) as a corrosion inhibitor for brass. First, the electrochemical measurements demonstrated a corrosion inhibition effect of MMI in a 3 wt.% NaCl solution. Next, the formation of the MMI surface layer and its properties after 1 month of immersion was analyzed with attenuated total reflectance–Fourier-transform infrared spectroscopy, atomic force microscopy, field-emission scanning electron microscopy, and contact angle analysis. Moreover, to gradually remove the organic surface layer, a gas cluster ion beam (GCIB) sputtering source at different accelerated voltages and cluster sizes was employed. After each sputtering cycle, a high-resolution XPS analysis was performed. Moreover, an angle‑resolved XPS analysis was carried out for the MMI-treated brass sample to analyze the heterogeneous layered structure (the interface of the MMI organic/inorganic brass substrate). The interface properties were also investigated in detail using ToF-SIMS for spectra measurements and 2D imaging. Special attention was devoted to the possible spectral interferences for MMI‑related species. The thermal stability of different MMI-related species using molecular-specific signals without possible spectral interferences was determined by performing a cooling/heating experiment associated with ToF-SIMS measurements. It was shown that these species desorbed from the brass surface in the temperature range of 310–370 °C.

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Mascali, David, Eugenia Naselli, and Giuseppe Torrisi. "Microwave techniques for electron cyclotron resonance plasma diagnostics." Review of Scientific Instruments 93, no. 3 (March 1, 2022): 033302. http://dx.doi.org/10.1063/5.0075496.

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This paper reviews the main microwave diagnostic techniques and tools adopted in electron cyclotron resonance (ECR) (and others) ion source laboratories, with a special focus on techniques and instruments developed at INFN-LNS. Along with the tools used for optimization of microwave launching (power monitors, spectral analysis, and network analyzers), this paper deals, in particular, with more recent devices on-purpose developed to perform in-plasma analysis, such as absolute density measurements and density profiles retrieval. Among these, the first example of microwave interferometry for ECR compact machines (the VESPRI interferometer at INFN-LNS) will be briefly discussed, in combination with microwave polarimetric techniques based on Faraday rotation detection. More sophisticated microwave techniques are going to be designed and are now at a numerical study stage, e.g., profilometry and imaging via inverse scattering methods (this paper will offer short theoretical bases and first numerical results on 1D profilometry). In the end, the relevance about the implications and interplays of microwave techniques in multidiagnostic systems (microwave, optical, and x-ray domains) will be commented, with a special focus on time resolved microwave measurements and advanced signal processing via wavelet transform, useful for characterization of plasma instabilities.

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Zachariassen, Linda G., Ljudmila Katchan, Anna G. Jensen, Darryl S. Pickering, Andrew J. R. Plested, and Anders S. Kristensen. "Structural rearrangement of the intracellular domains during AMPA receptor activation." Proceedings of the National Academy of Sciences 113, no. 27 (June 16, 2016): E3950—E3959. http://dx.doi.org/10.1073/pnas.1601747113.

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α-Amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptors (AMPARs) are ligand-gated ion channels that mediate the majority of fast excitatory neurotransmission in the central nervous system. Despite recent advances in structural studies of AMPARs, information about the specific conformational changes that underlie receptor function is lacking. Here, we used single and dual insertion of GFP variants at various positions in AMPAR subunits to enable measurements of conformational changes using fluorescence resonance energy transfer (FRET) in live cells. We produced dual CFP/YFP-tagged GluA2 subunit constructs that had normal activity and displayed intrareceptor FRET. We used fluorescence lifetime imaging microscopy (FLIM) in live HEK293 cells to determine distinct steady-state FRET efficiencies in the presence of different ligands, suggesting a dynamic picture of the resting state. Patch-clamp fluorometry of the double- and single-insert constructs showed that both the intracellular C-terminal domain (CTD) and the loop region between the M1 and M2 helices move during activation and the CTD is detached from the membrane. Our time-resolved measurements revealed unexpectedly complex fluorescence changes within these intracellular domains, providing clues as to how posttranslational modifications and receptor function interact.

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Henss, Anja, Marcus Rohnke, Thaqif El Khassawna, Parameswari Govindarajan, Gudrun Schlewitz, Christian Heiss, and Juergen Janek. "Applicability of ToF-SIMS for monitoring compositional changes in bone in a long-term animal model." Journal of The Royal Society Interface 10, no. 86 (September 6, 2013): 20130332. http://dx.doi.org/10.1098/rsif.2013.0332.

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Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a well-established technique in material sciences but has not yet been widely explored for implementation in life sciences. Here, we demonstrate the applicability and advantages of ToF-SIMS analysis for the study of minerals and biomolecules in osseous tissue. The locally resolved analysis of fragment ions deriving from the sample surface enables imaging and differentiation of bone tissue and facilitates histology on non-stained cross sections. In a rat model, bilateral ovariectomy combined with either a multi-deficiency diet or steroid treatment was carried out to create osteoporotic conditions. We focused our study on the Ca content of the mineralized tissue and monitored its decline. Calcium mass images of cross sections show the progressive degenerative changes in the bone. We observed a decreased Ca concentration in the edge region of the trabeculae and a decline in the Ca/P ratio. Additionally, we focused on the non-mineralized matrix and identified fragment ions that are characteristic for the collagen matrix. We observed trabeculae with wide ranges of non-mineralized collagen for the diet group owing to an impaired mineralization process. Here, the advantage of coeval monitoring of collagen and minerals indicated an osteomalacic model rather than an osteoporotic one.

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Kazak, Andrey, Kirill Simonov, and Victor Kulikov. "Machine-Learning-Assisted Segmentation of Focused Ion Beam-Scanning Electron Microscopy Images with Artifacts for Improved Void-Space Characterization of Tight Reservoir Rocks." SPE Journal 26, no. 04 (March 8, 2021): 1739–58. http://dx.doi.org/10.2118/205347-pa.

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Summary The modern focused ion beam-scanning electron microscopy (FIB-SEM) allows imaging of nanoporous tight reservoir-rock samples in 3D at a resolution up to 3 nm/voxel. Correct porosity determination from FIB-SEM images requires fast and robust segmentation. However, the quality and efficient segmentation of FIB-SEM images is still a complicated and challenging task. Typically, a trained operator spends days or weeks in subjective and semimanual labeling of a single FIB-SEM data set. The presence of FIB-SEM artifacts, such as porebacks, requires developing a new methodology for efficient image segmentation. We have developed a method for simplification of multimodal segmentation of FIB-SEM data sets using machine-learning (ML)-based techniques. We study a collection of rock samples formed according to the petrophysical interpretation of well logs from a complex tight gas reservoir rock of the Berezov Formation (West Siberia, Russia). The core samples were passed through a multiscale imaging workflow for pore-space-structure upscaling from nanometer to log scale. FIB-SEM imaging resolved the finest scale using a dual-beam analytical system. Image segmentation used an architecture derived from a convolutional neural network (CNN) in the DeepUNet (Ronneberger et al. 2015) configuration. We implemented the solution in the Pytorch® (Facebook, Inc., Menlo Park, California, USA) framework in a Linux environment. Computation exploited a high-performance computing system. The acquired data included three 3D FIB-SEM data sets with a physical size of approximately 20 × 15 × 25 µm with a voxel size of 5 nm. A professional geologist manually segmented (labeled) a fraction of slices. We split the labeled slices into training, validation, and test data. We then augmented the training data to increase its size. The developed CNN delivered promising results. The model performed automatic segmentation with the following average quality indicators according to test data: accuracy of 86.66%, precision of 54.93%, recall of 83.76%, and F1 score of 55.10%. We achieved a significant boost in segmentation speed of 14.5 megapixel (MP)/min. Compared with 0.18 to 1.45 MP/min for manual labeling, this yielded an efficiency increase of at least 10 times. The presented research work improves the quality of quantitative petrophysical characterization of complex reservoir rocks using digital rock imaging. The development allows the multiphase segmentation of 3D FIB-SEM data complicated with artifacts. It delivers correct and precise pore-space segmentation, resulting in little turn-around-time saving and increased porosity-data quality. Although image segmentation using CNNs is mainstream in the modern ML world, it is an emerging novel approach for reservoir-characterization tasks.

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Filotás, Dániel, Javier Izquierdo, Bibiana M. Fernández-Pérez, Lívia Nagy, Géza Nagy, and Ricardo M. Souto. "Contributions of Microelectrochemical Scanning Techniques for the Efficient Detection of Localized Corrosion Processes at the Cut Edges of Polymer-Coated Galvanized Steel." Molecules 27, no. 7 (March 27, 2022): 2167. http://dx.doi.org/10.3390/molecules27072167.

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Spatially resolved information on corrosion reactions operating at the cut edges of coated metals can be obtained using microelectrochemical scanning techniques using a suitable selection of operation modes and scanning probes. The scanning vibrating electrode technique (SVET) provides current density maps with a spatial resolution of the order of the dimensions of the sample, which allows the temporal evolution of the corrosion reactions to be followed over time. This leads to the identification and localization of cathodic and anodic sites, although the technique lacks chemical specificity for the unequivocal identification of the reactive species. The application of scanning electrochemical microscopy (SECM) was previously limited to image cathodic reaction sites, either due to oxygen consumption in the amperometric operation or by the alkalinisation of the electrolyte in potentiometric operation. However, it is shown that anodic sites can be effectively monitored using an ion-selective microelectrode (ISME) as a probe. The ISME probes detected differences in the local concentrations of Zn2+ and OH− ions from the cut edges of a complete coil coating system compared to the same system after the polymeric layers were removed. In this way, it has been shown that the inhibitor loading in the polymer layers effectively contributes to reducing the corrosion rates at the cut edge, thus helping to extend the useful life of the sacrificial galvanized layer bonded directly to the steel matrix. Additionally, these two probe configurations can be integrated into a multi-electrode tip for potentiometric operation to simultaneously monitor localized changes in pH values and metal ion dissolution in a single scan. Spatial and temporal distributions were further investigated using different rastering procedures, and the potential of constructing pseudomaps for 2D-imaging is described.

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Veyrinas, K., V. Gruson, S. J. Weber, L. Barreau, T. Ruchon, J. F. Hergott, J. C. Houver, R. R. Lucchese, P. Salières, and D. Dowek. "Molecular frame photoemission by a comb of elliptical high-order harmonics: a sensitive probe of both photodynamics and harmonic complete polarization state." Faraday Discussions 194 (2016): 161–83. http://dx.doi.org/10.1039/c6fd00137h.

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Due to the intimate anisotropic interaction between an XUV light field and a molecule resulting in photoionization (PI), molecular frame photoelectron angular distributions (MFPADs) are most sensitive probes of both electronic/nuclear dynamics and the polarization state of the ionizing light field. Consequently, they encode the complex dipole matrix elements describing the dynamics of the PI transition, as well as the three normalized Stokes parameters s₁, s₂, s₃ characterizing the complete polarization state of the light, operating as molecular polarimetry. The remarkable development of advanced light sources delivering attosecond XUV pulses opens the perspective to visualize the primary steps of photochemical dynamics in time-resolved studies, at the natural attosecond to few femtosecond time-scales of electron dynamics and fast nuclear motion. It is thus timely to investigate the feasibility of measurement of MFPADs when PI is induced e.g., by an attosecond pulse train (APT) corresponding to a comb of discrete high-order harmonics. In the work presented here, we report MFPAD studies based on coincident electron-ion 3D momentum imaging in the context of ultrafast molecular dynamics investigated at the PLFA facility (CEA-SLIC), with two perspectives: (i) using APTs generated in atoms/molecules as a source for MFPAD-resolved PI studies, and (ii) taking advantage of molecular polarimetry to perform a complete polarization analysis of the harmonic emission of molecules, a major challenge of high harmonic spectroscopy. Recent results illustrating both aspects are reported for APTs generated in unaligned SF₆ molecules by an elliptically polarized infrared driving field. The observed fingerprints of the elliptically polarized harmonics include the first direct determination of the complete s₁, s₂, s₃ Stokes vector, equivalent to (ψ, ε, P), the orientation and the signed ellipticity of the polarization ellipse, and the degree of polarization P. They are compared to so far incomplete results of XUV optical polarimetry. We finally discuss the comparison between the outcomes of photoionization and high harmonic spectroscopy for the description of molecular photodynamics.

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Pham, Martin T. M., Donal P. Finegan, John J. Darst, Gareth Hinds, Eric Darcy, and Paul R. Shearing. "Prevention, Mitigation and Correlative Acoustic Spectroscopy of Lithium-Ion Battery Thermal Runaway." ECS Meeting Abstracts MA2022-01, no. 2 (July 7, 2022): 435. http://dx.doi.org/10.1149/ma2022-012435mtgabs.

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Scrutiny of lithium-ion battery failure has seen heavy regulations and restrictions with well-reported headlines of catastrophic thermal runaway of commercial electronic devices and electric vehicles. Thermal runaway occurs at a critical temperature when the rate of heat generation exceeds that of dissipation, highly exothermic decomposition reactions occur and temperatures in excess of 600 ᵒC can be measured 1. These concerns continue to grow with applications of greater energy density and capacity, such as the proliferation of electric vehicles. Isolation of electronically conductive components within the electrode assembly to prevent short circuit has shown promise to prevent the onset of thermal runaway within lithium-ion cells. Here 2, the authors present a metal-coated polymer current collector (PCC) and thermally stable separator (TSS) to prevent and mitigate thermal runaway. 2.10 Ah capacity 18650-geometry cells were subject to thermal, internal short circuit and nail penetration abuse techniques with these materials and their commercial counterparts for individual comparison of the PCCs and TSS. Reductions in cell mass were observed on the order of 5%, due to the majority of the PCC consisting of the polymer substrate rather than pure aluminium and copper in commercial current collectors. High speed synchrotron facilities provided insights into the function of the polymer current collectors with post- mortem X-ray computed tomography. During mitigation testing, cells were taken to failure with thermal and with an internal short circuit device (ISCD) within a Fraction Thermal Runaway Calorimeter (FTRC) to measure the reduction in calorific output. This highlighted the difficulty that exists with detecting gas-induced and internal structural degradation within lithium-ion batteries, especially outside specialized diagnostic laboratories to characterize these rapid changes with elapse within seconds. Attenuation and wave velocity determined by the propagative properties of ultrasound through different phases, prominently highlights structural, temperature and formation of different phases which occur during thermal runaway. Such analysis provided by acoustic spectroscopy are characterised by variations in the attenuation and signal peak shifts. Further information which can be derived from spatial mapping using acoustic spectroscopy 3,4 include: state of charge, state of health, electrochemical performance. Cells made with the aluminium-coated PCC demonstrated 100% success in prevention of thermal runaway during nail penetration, retaining a voltage above 4.00 V. Cells manufactured with the PCC, both PCC and TSS, exhibited a reduction in total energy output on average of 19.4% and 41.3% respectively during thermal abuse. ISCD triggered thermal runaways also observed reductions of 24.6% and 30.3% with these respective cell material configurations. Prevention of thermal runaway is a transformative advancement in improving lithium-ion battery safety, especially in the cylindrical 18650-format cell. Additionally, significant reductions in the calorific output during failure were measured. These safety innovations provides efficacy of these materials independent of cell chemistry (provided they are stable in the operating environment) while also increasing the energy density and be assimilated into existing manufacturing technology. Furthermore, the authors demonstrate correlative high-speed acoustic spectroscopy during routine cycling of a commercial 210 mAh lithium-ion pouch cell and during thermal abuse 5. Mechanical deformation such as gas-induced delaminations, which have been linked to degradation in electrochemical performance, capacity retention, cell state of health and impending thermal runaway, were detected. This degradation was observed with characteristic acoustic spectroscopy signal peaks changes during cycling due to cell manufacturing defects and during induced thermal abuse, were corroborated with high speed synchrotron X-ray imaging. This analysis can be observed immediately after application of the acoustic probe which emphasises the rapid diagnostics insights provided by acoustic spectroscopy as a robust field deployable technique. Thus, integration into battery management systems, second-life evaluation/recycling or as in-line cell metrology during manufacturing would provide real time direct insight into these metrics. Finegan DP, Darcy E, Keyser M, et al. Identifying the Cause of Rupture of Li-Ion Batteries during Thermal Runaway. Adv Sci. 2018. doi:10.1002/advs.201700369 Pham MTM, Darst JJ, Walker WQ, et al. Prevention of lithium-ion battery thermal runaway using polymer-substrate current collectors. Cell Reports Phys Sci. 2021. doi:10.1016/j.xcrp.2021.100360 Robinson JB, Pham M, Kok MDR, Heenan TMM, Brett DJL, Shearing PR. Examining the Cycling Behaviour of Li-Ion Batteries Using Ultrasonic Time-of-Flight Measurements. J Power Sources. 2019;444. Robinson JB, Maier M, Compton T, Alster G, Brett DJL, Shearing PR. Spatially resolved ultrasound diagnostics of Li-ion battery electrodes. Phys Chem Chem Phys. 2018. doi:10.1039/c8cp07098a Pham MTM, Darst JJ, Finegan DP, et al. Correlative acoustic time-of-flight spectroscopy and X-ray imaging to investigate gas-induced delamination in lithium-ion pouch cells during thermal runaway. J Power Sources. 2020;470:228039. doi:10.1016/j.jpowsour.2020.228039

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Das, Sushanta K., Navaneetha K. Subbaiyan, Francis D'Souza, Atula S. D. Sandanayaka, Takatsugu Wakahara, and Osamu Ito. "Formation and photoinduced properties of zinc porphyrin-SWCNT and zinc phthalocyanine-SWCNT nanohybrids using diameter sorted nanotubes assembled via metal-ligand coordination and π–π stacking." Journal of Porphyrins and Phthalocyanines 15, no. 09n10 (September 2011): 1033–43. http://dx.doi.org/10.1142/s1088424611003951.

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Photoinduced electron transfer processes in self-assembled zinc porphyrin ( ZnP ) or zinc phthalocyanine ( ZnPc ) with semiconducting (7,6)- and (6,5)-enriched SWCNTs were investigated. To bind photosensitizers to SWCNTs, first, pyrene covalently functionalized with a phenylimidazole (Im-Pyr) entity was treated with SWCNTs. Exfoliation of SWCNTs occurred due to π–π stacking of pyrene with nanotubes walls leaving the imidazole entity that was subsequently used to coordinate ZnP or ZnPc in o-dichlorobenzene (DCB). The donor-acceptor nanohybrids thus formed were characterized by TEM imaging, steady-state UV-visible-near IR absorption and fluorescence spectra. Free-energy calculations suggested possibility of electron transfer from the photoexcited ZnP or ZnPc to Im-Pyr/SWCNT(n,m) in the nanohybrids. Consequently, steady-state and time-resolved fluorescence studies revealed efficient quenching of the singlet excited state of ZnP or ZnPc with the rate constants of charge separation (k CS ) in the range of (3–6) × 109 s-1. Nanosecond transient absorption technique confirmed the electron transfer products, ZnP·+←Im-Pyr/SWCNT·- and ZnPc·+←Im-Pyr/SWCNT·- (and opposite charged pairs) having characteristic absorptions with the decay rate constants due to charge recombination (k CR ) in the range of (1.4–2.4) × 107 s-1, corresponding to lifetimes of radical ion-pairs in the 70–100 ns range. The SWCNT·- was further utilized to mediate electrons to hexyl-viologen dication (HV2+) resulting in an electron-accumulation process in the presence of sacrificial electron donor, offering additional proof for the occurrence of photoinduced charge-separation and potential utilization of these materials in light energy harvesting applications. Further, photoelectrochemical cells have been constructed on FTO/ SnO2 electrodes to verify their ability to directly convert light into electricity. An IPCE efficiency of up to 7% has been achieved in case of ZnP←Im-Pyr/SWCNT modified electrode.

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Deitz, Julia, Timothy Ruggles, Stephen Lee, Andrew A. Allerman, C. Barry Carter, and Joseph Michael. "(Invited) Electron Channeling Contrast Imaging for Rapid Characterization of Compound Semiconductors." ECS Meeting Abstracts MA2022-02, no. 34 (October 9, 2022): 1254. http://dx.doi.org/10.1149/ma2022-02341254mtgabs.

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As compound semiconductor devices become more advanced, their ultimate performance becomes increasingly dependent on nano to micro scale structural defects in their constituent materials. These defects, such as dislocations, stacking faults, and anti-phase boundaries often act as recombination centers in devices, limiting efficiency. Characterization of these defects – their type (such as edge vs. screw vs. mixed dislocations), their relative densities, how they interact with other defects, what growth conditions are more or less likely to propagate them, how they relate to device efficiencies and performance, etc. – is vital to mitigate their negative effects and even sometimes exploit their potential benefits depending on the desired application. In this contribution, we will discuss the use of electron channeling contrast imaging (ECCI) as an ideal characterization method for compound semiconductors and devices as well as some recent applications which include ECCI characterization in tandem with other characterization methods for a broader material understanding. Transmission electron microscopy (TEM) is a widely used technique for characterizing extended defects and local crystal orientation. However, TEM analysis usually entails thinning a sample via focused ion beam milling or chemical/mechanical polishing to around 50-100 nm, which is time consuming and only allows a relatively small area of the sample to be characterized. These drawbacks can cause bottlenecks in research progress and even render TEM impractical for certain applications. ECCI performed in a scanning electron microscope (SEM) can bypass these issues as it requires little to no sample preparation. This means ECCI can easily characterize over large areas in a fraction of the time as TEM analysis. [1-3] These benefits mean that ECCI gives more accurate analysis by not missing larger trends that can be missed with the small samples in TEM as well as by not introducing artifacts from the sample preparation. Here we highlight applications of ECCI for characterization of two very different compound semiconductors of growing importance -- Cd3As2 and GaN. Firstly, we consider Cd3As2 thin films of use as topological quantum materials, where the Cd3As2 can be either a compound semiconductor or topological Dirac semimetal, depending on the structural phase or mode of use. The ECCI of MOCVD-grown Cd3As2 shown in this work finds that the developmental thin films are not completely single crystalline. [4] Moreover, two different spatial scales of domain formation are seen. At lower magnification, we see roughly circular-shaped larger domains that are ~ 2-5 mm in diameter. Some of these domains are more prominently defined and feature single dark spots at their center, which at first suggests threading dislocations, but turns out to be occasional defect-pits formed in concert with numerous, indistinct threads. At higher magnification, we see much smaller dot-like or speck-like domains that are ~ 100 nm or less in diameter. The wide-area electron channeling patterns used to orient the sample for the ECCI imaging were visible, but rather indistinctly resolved, which is consistent with small crystallographic misorientations of the ensemble of domains composing the film. Secondly, we consider bulk GaN wafers entering use in a wide variety of functional applications, including GaN high-voltage diodes for power electronics. We will show novel “star” defects appearing in the GaN substrates when characterized by both ECCI and high-resolution electron backscattered diffraction (EBSD). [5] Through a more complete structural understanding of these star defects, we seek to improve understanding of the impact of these defects on device performance, which may in turn facilitate development of strategies for their mitigation or removal. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525.

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Ramey, Nicholas A., Mark J. Lucarelli, Lindell R. Gentry, and Cat N. Burkat. "Clinical Usefulness of Orbital and Facial Time-Resolved Imaging of Contrast KineticS (TRICKS) Magnetic Resonance Angiography." Ophthalmic Plastic and Reconstructive Surgery 28, no. 5 (2012): 361–68. http://dx.doi.org/10.1097/iop.0b013e318261161e.

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Hack, Jennifer, Yiyang Liu, Toby Neville, Hongzhen He, Guanjie He, Paul R. Shearing, and Dan Brett. "Characterisation of Anode Morphology Evolution in Zinc-Air Batteries." ECS Meeting Abstracts MA2022-01, no. 1 (July 7, 2022): 19. http://dx.doi.org/10.1149/ma2022-01119mtgabs.

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With the urgent need to move away from fossil fuels towards more sustainable technologies, alternative battery technologies are needed to alleviate the existing supply and safety concerns associated with Li-ion batteries1. Metal-air batteries are one such alternative that hold promise thanks to their high theoretical specific energies2. Whilst zinc-air batteries have one of the lowest theoretical specific energies (~1350 Wh kg-1 for zinc-air versus 5200 Wh kg-1 for Li-air2), zinc is an abundant element and there are few safety concerns associated with this type of battery. Furthermore, the theoretical specific energy of a zinc-air cell is still around three times higher than Li-ion (upwards of 270 Wh kg-1)3. Currently, primary zinc-air cells are commercialised for application in hearing aids, but the commercialisation of secondary cells is still limited by poor cycle lifetimes and degradation of the anode4. Thus, alongside the need to develop better bifunctional catalysts, improvements need to be made to the anode to avoid dendrite formation and improve the reversibility between zinc and zinc oxide (ZnO) during cycling; there is significant volume expansion and morphology change during reaction from zinc to ZnO. In order to visualise the changes occurring in zinc-air battery electrodes, X-ray computed tomography (CT) has been used in a number of studies5-7. It is non-destructive and internal features of the sample can be visualised and measured without the need to open the sample. This allows for time-resolved quantification of changes occurring to the various phases within zinc-air cells, like zinc or ZnO. In this work, we explore the morphologies of different anode electrode types, including foils, free-standing electrodes and slurries, to highlight the various existing anode design concepts for secondary zinc-air cells. Imaging methods, including X-ray CT and scanning electron microscopy (SEM), are used to visualise the structure of these electrodes, and quantitative analysis allows for the morphology to be correlated to their electrochemical performance. We discuss the advantages and disadvantages of the different electrode types and, finally, share our perspectives on the future of anode design for zinc-air cells. References 1Y. Hau, X. Liu, S. Zhou, Y. Huang, H. Ling and S. Yang, Resour. Conserv. Recycl., 2021, 168, 105249. 2M. A. Rahman, X. Wang and C. Wen, J. Electrochem. Soc., 2013, 160, A1759-A1771. 3J. -S. Lee, S. Tai Kim, R. Cao, N. -S. Choi, M. Liu, K. T. Lee and J. Cho, Adv. Energy Mater., 2011, 1, 34-50. 4J. Zhang, Q. Zhou, Y. Tang, L. Zhang and Y. Li, Chem. Sci., 2019, 10, 8924-8929. 5T. Arlt, D. Schröder, U. Krewer and I. Manke, Phys. Chem. Chem. Phys, 2014, 16, 22273-22280. 6J. Hack, D. Patel, J. J. Bailey, F. Iacoviello, P. R. Shearing and D. J. L. Brett, J. Phys: Mater., https://doi.org/10.1088/2515-7639/ac3f9a. 7B. Bozzini, C. Mele, A. Veneziano, N. Sodini, G. Lanzafame, A. Taurino and L. Mancini, ACS Appl. Energy Mater., 2020, 3, 4931-4940. Figure 1

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Watanabe, Y., K. Endo, and H. Sano. "Short-lived chemical species of57Fe in57Co-labelled Co/IO3/2 studied by time-resolved emission Mössbauer spectroscopy." Journal of Radioanalytical and Nuclear Chemistry Letters 119, no. 6 (December 1987): 467–76. http://dx.doi.org/10.1007/bf02261209.

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Khodadoust, Michael, Alain H. Rook, Pierluigi Porcu, Francine M. Foss, Alison J. Moskowitz, Andrei R. Shustov, Satish Shanbhag, et al. "Pembrolizumab for Treatment of Relapsed/Refractory Mycosis Fungoides and Sezary Syndrome: Clinical Efficacy in a Citn Multicenter Phase 2 Study." Blood 128, no. 22 (December 2, 2016): 181. http://dx.doi.org/10.1182/blood.v128.22.181.181.

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Abstract Background:PD-1 and PD-L1/PD-L2 are expressed by malignant T-cells in mycosis fungoides (MF) and Sézary syndrome (SS). PD-1 is additionally expressed by tumor-infiltrating cytotoxic T-cells and PD-L1 is expressed by macrophages and other stromal components of the tumor microenvironment in these diseases. Moreover, reports of 9p24.1/PD-L2 translocation and CTLA4-CD28 fusion events in MF/SS support a genomic basis for immune evasion. Here, we explore the clinical activity of pembrolizumab, an immune checkpoint inhibitor of the PD-1/PD-L1 axis, in MF/SS. Methods:Patients (pts) with MF/SS stages IB-IV treated with at least 1 prior systemic therapy were enrolled in this phase 2, single-arm study coordinated by the Cancer Immunotherapy Trials Network (CITN). A Simon two-stage design was applied where stage 2 is initiated if 1 of 9 pts had an objective response. An additional 15 pts were planned in stage 2. Pembrolizumab was administered at 2 mg/kg every 3 weeks and treatment was allowed up to 2 years. The primary endpoint was overall response rate (ORR) as determined by the consensus global response criteria. Secondary endpoints were safety/tolerability, time to response (TTR), duration of response (DOR) and progression-free survival (PFS). Correlative biomarker studies included immunohistochemistry (IHC) staining for PD-L1, PD-L2, and multiple immune subsets as well as serum analysis of 62 cytokines and chemokines. Phenotypic and functional profiling of malignant and non-malignant immune cells will be performed by flow cytometry and mass cytometry (CyTOF). Results: The study completed enrollment and all 24 patients received at least one dose of pembrolizumab. Median age was 67 (range 44-85); 18 were male. Patients were advanced stage with 23 patients (96%) stage IIB or higher, including 15 patients (63%) with stage IVA SS. Most pts were heavily treated with a median of 4 prior systemic therapies (range 1-11). The median follow-up time was 40 weeks (range 9-60 weeks). The objective response rate (ORR) was 38% with 1 complete response (CR) and 8 partial responses (PR). Of the responding pts, 6 pts had 90% or greater improvement in skin disease as measured by mSWAT. An additional 9 pts (38%) had stable disease (SD). The median TTR was 11 weeks (range 8-41 weeks). Responses were durable with 8 of 9 (89%) responses currently ongoing at a median of 32 weeks of duration (4-46). The median PFS has not yet been reached, and the one-year PFS was 69%. There was no significant association between response and clinical characteristics including stage, disease type (MF vs. SS), and number of prior therapies, nor with skin tissue expression of PD-1, PD-L1, PD-L2, or infiltrating CD8+ T-cells as determined by IHC. Planned additional correlatives including CyTOF profiling, gene expression profiling, T cell receptor high throughput sequencing, multiplexed ion beam imaging (MIBI), and whole exome sequencing will explore potential predictive biomarkers of response. Adverse events (AE) were consistent with those seen in prior studies of pembrolizumab with the exception of an immune-mediated skin flare reaction seen in 6 pts (2 grade 2 and 4 grade 3). Skin flares occurred exclusively in patients with SS (6/15; 40%) and were associated with lower serum levels of the cytokines IL-7 and SCF prior to pembrolizumab treatment (p=0.01 and p=0.02 respectively, n.s. by Bonferroni correction). Pts with the skin flare reaction experienced increases in serum IFN-gamma, IL-12p40, IL-15, LIF, G-CSF, and CCL4 following treatment. There were two treatment related serious adverse events (SAE), both immune related. One pt experienced grade 2 pneumonitis which resolved with systemic corticosteroids. Another patient experienced grade 3 diarrhea secondary to steroid-refractory duodenitis. Conclusions: Pembrolizumab has significant clinical activity in pts with previously treated MF/SS. Responses were durable and were not associated with any identifiable clinical or pathologic characteristics. Treatment was well tolerated with a toxicity profile consistent with prior pembrolizumab studies, though 40% of pts with SS developed a notable skin flare reaction. These findings support further study of PD-1 blockade in the treatment of MF and SS. A phase 2 trial of pembrolizumab in combination with interferon-gamma is being developed based on these results. Disclosures Porcu: Millenium: Other: investigator in a clinical trial; miRagen: Other: Investigator in a clinical trial; celgene: Other: Investigator in a clinical trial; Innate Pharma: Other: Investigator in a clinical trial. Foss:Celgene: Consultancy, Research Funding, Speakers Bureau; Eisai: Consultancy; Seattle Genetics: Consultancy, Speakers Bureau; Spectrum Pharmaceuticals: Consultancy. Moskowitz:Bristol Myers Squibb: Honoraria; Merck: Honoraria; Seattle Genetics: Honoraria, Research Funding. Sokol:Seattle Genetics: Consultancy; Spectrum: Consultancy. Yearley:Merck: Employment. Chartash:Merck: Employment. Townson:Merck: Employment. Horwitz:Spectrum: Consultancy, Research Funding; Bristol-Myers Squibb: Consultancy; Huya: Consultancy; Infinity: Consultancy, Research Funding; Kyowa Hakka Kirin: Consultancy, Research Funding; Takeda: Consultancy, Research Funding; Seattle Genetics: Consultancy, Research Funding; Celgene: Consultancy; ADCT Therapeutics: Research Funding. Kim:Seattle Genetics: Consultancy, Other: Investigator in a clinical trial; Merck: Other: Investigator in a clinical trial; Neumedicine: Consultancy; Soligenix: Consultancy; Galderma: Consultancy; Genentech: Other: Investigator in a clinical trial; Innate Pharma: Other: Investigator in a clinical trial; Kyowa Hakko Kirin: Consultancy, Honoraria, Other, Research Funding; Millenium: Consultancy, Other: Investigator in a clinical trial; Eisai: Consultancy, Other: Investigator in a clinical trial; Actelion: Consultancy, Other: Investigator in a clinical trial; Celgene: Consultancy; MiRagen: Consultancy; Horizon: Consultancy.

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Journal articles on the topic 'TIME-RESOLVED ION IMAGING'

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