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At least 307 records · Page 17

Electronic signatures of Lorentzian dynamics and charge fluctuations in lithiated graphite structures

Lithium graphite intercalation compounds (Li-GICs) are essential materials for modern day portable electronics and obtaining insights into their atomic structure and thermodynamics is of fundamental interest. Here we explore the electronic and atomic states of Li-GICs at varying degrees of Lithium loading (i.e., “staging”) by means of ab-initio molecular dynamics simulations and simulated X-ray adsorption spectroscopy (XAS). We analyze the atomic correlation functions and shows that the enhancements of the Li-ion entropy with increased staging result from Lorentzian lithium-ion dynamics and charge fluctuations, which activate low-energy phonon modes. The associated electronic signatures are modulations of the unoccupied π*/σ* orbital energy levels and unambiguous fingerprints in Carbon K-edge XAS spectra. Thus, we extend the canonical view of XAS, establishing that these “static” measurements in fact encode the signature of the thermodynamic response and relaxation dynamics of the system. This causal link between atomic structure, spectroscopy, thermodynamics, and information theory can be generally exploited to better understand stability in solid-state electrochemical systems.

25 ENERGY STORAGE↗

Active species in chloroaluminate ionic liquids catalyzing low-temperature polyolefin deconstruction

Abstract Chloroaluminate ionic liquids selectively transform (waste) polyolefins into gasoline-range alkanes through tandem cracking-alkylation at temperatures below 100 °C. Further improvement of this process necessitates a deep understanding of the nature of the catalytically active species and the correlated performance in the catalyzing critical reactions for the tandem polyolefin deconstruction with isoalkanes at low temperatures. Here, we address this requirement by determining the nuclearity of the chloroaluminate ions and their interactions with reaction intermediates, combining in situ 27 Al magic-angle spinning nuclear magnetic resonance spectroscopy, in situ Raman spectroscopy, Al K-edge X-ray absorption near edge structure spectroscopy, and catalytic activity measurement. Cracking and alkylation are facilitated by carbenium ions initiated by AlCl 3 - tert -butyl chloride (TBC) adducts, which are formed by the dissociation of Al 2 Cl 7 − in the presence of TBC. The carbenium ions activate the alkane polymer strands and advance the alkylation cycle through multiple hydride transfer reactions. In situ 1 H NMR and operando infrared spectroscopy demonstrate that the cracking and alkylation processes occur synchronously; alkenes formed during cracking are rapidly incorporated into the carbenium ion-mediated alkylation cycle. The conclusions are further supported by ab initio molecular dynamics simulations coupled with an enhanced sampling method, and model experiments using n-hexadecane as a feed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Probing the interplay between lattice dynamics and short-range magnetic correlations in CuGeO 3 with femtosecond RIXS

Investigations of magnetically ordered phases on the femtosecond timescale have provided significant insights into the influence of charge and lattice degrees of freedom on the magnetic sub-system. However, short-range magnetic correlations occurring in the absence of long-range order, for example in spin-frustrated systems, are inaccessible to many ultrafast techniques. Here, we show how time-resolved resonant inelastic X-ray scattering (trRIXS) is capable of probing such short-ranged magnetic dynamics in a charge-transfer insulator through the detection of a Zhang–Rice singlet exciton. Utilizing trRIXS measurements at the O K-edge, and in combination with model calculations, we probe the short-range spin correlations in the frustrated spin chain material CuGeO 3 following photo-excitation, revealing a strong coupling between the local lattice and spin sub-systems.

36 MATERIALS SCIENCE↗

Revealing key structures for reversible sulfur redox in amorphous polymeric sulfur

Amorphous polymeric sulfur cathodes, such as sulfurized polyacrylonitrile (SPAN), enable high-energy lithium-sulfur batteries without cobalt or nickel, leveraging abundant sulfur. However, the limited in situ understanding of their synthesis and electrochemistry has impeded targeted optimization. Here, in this study, we integrate operando high-energy total scattering with sulfur K-edge X-ray absorption spectroscopy to monitor SPAN's formation and cycling in real time. Our results show that S-C bond formation halts further fusion of cyclized polyacrylonitrile, fostering π-π stacking and a transition from long-chain to short-chain sulfur-critical for reversible sulfur redox. These features synergistically minimize polysulfide dissolution and charge-transfer resistance, enabling optimized SPAN to achieve high capacity retention over 1,000 cycles. Operando X-ray absorption spectroscopy reveals that residual protons drive thiol-thione tautomerism, with lithium replacement during the first discharge causing ~20% irreversible capacity loss. To enhance performance, minimizing -NH groups and expanding pyridine networks are key. These findings transform SPAN optimization from empirical tuning to mechanism‑guided engineering and point the way towards sulfur loadings and energy densities competitive with state‑of‑the‑art Li‑ion cathodes.

25 ENERGY STORAGE↗

Dispersion and stability mechanism of Pt nanoparticles on transition-metal oxides

The heterogeneous catalysts of Pt/transition-metal oxides are typically synthesized through calcination at 500 °C, and Pt nanoparticles are uniformly and highly dispersed when hydrogen peroxide (H 2 O 2 ) is applied before calcination. The influence of H 2 O 2 on the dispersion and the stability of Pt nanoparticles on titania-incorporated fumed silica (Pt/Ti–FS) supports was examined using X-ray absorption fine structure (XAFS) measurements at the Pt L 3 and Ti K edges as well as density functional theory (DFT) calculations. The local structural and chemical properties around Pt and Ti atoms of Pt/Ti–FS with and without H 2 O 2 treatment were monitored using in-situ XAFS during heating from room temperature to 500 °C. XAFS revealed that the Pt nanoparticles of H 2 O 2 -Pt/Ti–FS are highly stable and that the Ti atoms of H 2 O 2 -Pt/Ti–FS support form into a distorted-anatase TiO 2 . DFT calculations showed that Pt atoms bond more stably to oxidized–TiO 2 surfaces than they do to bare- and reduced–TiO 2 surfaces. XAFS measurements and DFT calculations clarified that the presence of extra oxygen atoms due to the H 2 O 2 treatment plays a critical role in the strong bonding of Pt atoms to TiO 2 surfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hard X-ray inverse Compton scattering at photon energy of 87.5 keV

Abstract Production of hard X-ray via inverse Compton scattering at photon energies below 100 keV range aimed at potential applications in medicine and material research is reported. Experiments have been performed at the Brookhaven National Laboratory, Accelerator Test Facility, employing the counter collision of a 70 MeV, 0.3 nC electron beam with a near infra-red Nd: YAG laser (1064 nm wavelength) pulse containing ~ 100 mJ in a single shot basis. The radiation distribution of the scattered photon beam is assessed to be sufficiently quasi monochromatic to produce clear contrast from the Au K - edge at 80.7 keV.

43 PARTICLE ACCELERATORS↗

Local lattice distortions drive the transition of BaIrO 3 into a ferromagnetic insulator state

Using variable temperature total and resonant x-ray scattering at the K edge of Ir species, we study the “bad metal” to insulator transition in BaIrO 3 , a canonical third transition series oxide. The usage of advanced experimental techniques and large-scale computer modeling helps us show that, contrary to the widely accepted view, charge disproportionation leading to the formation of Ir-trimers with a different number of 5d valence electrons already exists at room temperature. The charge disbalance between the trimers does not evolve much with decreasing temperature while local lattice distortions do, suggesting that the latter and not the former make a key contribution to the emergence of the enigmatic ferromagnetic insulator state of BaIrO 3 . The conclusion is supported by DFT calculations based on unmodified experimental structure data. Our work calls for a reconsideration of the role of lattice distortions in determining the electronic properties of third transition series oxides. It also charts a path to assessing these properties on a realistic and not assumed crystal structure basis.

36 MATERIALS SCIENCE↗

Site-specific interrogation of an ionic chiral fragment during photolysis using an X-ray free-electron laser

Abstract Short-wavelength free-electron lasers with their ultrashort pulses at high intensities have originated new approaches for tracking molecular dynamics from the vista of specific sites. X-ray pump X-ray probe schemes even allow to address individual atomic constituents with a ‘trigger’-event that preludes the subsequent molecular dynamics while being able to selectively probe the evolving structure with a time-delayed second X-ray pulse. Here, we use a linearly polarized X-ray photon to trigger the photolysis of a prototypical chiral molecule, namely trifluoromethyloxirane (C 3 H 3 F 3 O), at the fluorine K-edge at around 700 eV. The created fluorine-containing fragments are then probed by a second, circularly polarized X-ray pulse of higher photon energy in order to investigate the chemically shifted inner-shell electrons of the ionic mother-fragment for their stereochemical sensitivity. We experimentally demonstrate and theoretically support how two-color X-ray pump X-ray probe experiments with polarization control enable XFELs as tools for chiral recognition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Extended X-ray absorption spectroscopy using an ultrashort pulse laboratory-scale laser-plasma accelerator

Laser-driven compact particle accelerators can provide ultrashort pulses of broadband X-rays, well suited for undertaking X-ray absorption spectroscopy measurements on a femtosecond timescale. Here the Extended X-ray Absorption Fine Structure (EXAFS) features of the K-edge of a copper sample have been observed over a 250 eV window in a single shot using a laser wakefield accelerator, providing information on both the electronic and ionic structure simultaneously. This capability will allow the investigation of ultrafast processes, and in particular, probing high-energy-density matter and physics far-from-equilibrium where the sample refresh rate is slow and shot number is limited. For example, states that replicate the tremendous pressures and temperatures of planetary bodies or the conditions inside nuclear fusion reactions. Using high-power lasers to pump these samples also has the advantage of being inherently synchronised to the laser-driven X-ray probe. A perspective on the additional strengths of a laboratory-based ultrafast X-ray absorption source is presented.

43 PARTICLE ACCELERATORS↗

Quantitative temporally and spatially resolved X-ray fluorescence microprobe characterization of the manganese dissolution-deposition mechanism in aqueous Zn/α-MnO 2 batteries

Rechargeable aqueous Zn/α-MnO 2 batteries are a possible alternative to lithium ion batteries for scalable stationary energy storage applications due to their low cost, safety and environmentally benign components. A critical need for advancement of this battery system is a full understanding of the electrochemical reaction mechanisms, which remain unclear. In this report, operando , spatiotemporal resolved synchrotron X-ray fluorescence mapping measurements on a custom aqueous Zn/α-MnO 2 cell provided direct evidence of a Mn dissolution-deposition faradaic mechanism that governs the electrochemistry. Simultaneous visualization and quantification of the Mn distribution in the electrolyte revealed the formation of aqueous Mn species during discharge and depletion on charge. The findings are supported by ex situ transmission electron microscopy (TEM), X-ray diffraction, Mn K-edge X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) measurements. The elucidated mechanism is fundamentally different from the previously proposed Zn 2+ insertion or conversion reactions. These findings provide a foundation for developing dissolution- deposition chemistries suitable for scalable stationary energy storage with aqueous electrolyte.

25 ENERGY STORAGE↗

Single-ion magnetism in the extended solid-state: insights from X-ray absorption and emission spectroscopy

Large single-ion magnetic anisotropy is observed in lithium nitride doped with iron. The iron sites are two-coordinate, putting iron doped lithium nitride amongst a growing number of two coordinate transition metal single-ion magnets (SIMs). Uniquely, the relaxation times to magnetisation reversal are over two orders of magnitude longer in iron doped lithium nitride than other 3d-metal SIMs, and comparable with high-performance lanthanide-based SIMs. To understand the origin of these enhanced magnetic properties a detailed characterisation of electronic structure is presented. Access to dopant electronic structure calls for atomic specific techniques, hence a combination of detailed single-crystal X-ray absorption and emission spectroscopies are applied. Together K-edge, L 2,3 -edge and Kβ X-ray spectroscopies probe local geometry and electronic structure, identifying iron doped lithium nitride to be a prototype, solid-state SIM, clean of stoichiometric vacancies where Fe lattice sites are geometrically equivalent. Extended X-ray absorption fine structure and angular dependent single-crystal X-ray absorption near edge spectroscopy measurements determine Fe I dopant ions to be linearly coordinated, occupying a D 6h symmetry pocket. The dopant engages in strong 3dπ-bonding, resulting in an exceptionally short Fe–N bond length (1.873(7) Å) and rigorous linearity. It is proposed that this structure protects dopant sites from Renner–Teller vibronic coupling and pseudo Jahn–Teller distortions, enhancing magnetic properties with respect to molecular-based linear complexes. The Fe ligand field is quantified by L 2,3 -edge XAS from which the energy reduction of 3d z 2 due to strong 4s mixing is deduced. Quantification of magnetic anisotropy barriers in low concentration dopant sites is inhibited by many established methods, including far-infrared and neutron scattering. We deduce variable temperature L 3 -edge XAS can be applied to quantify the J = 7/2 magnetic anisotropy barrier, 34.80 meV (~280 cm –1 ), that corresponds with Orbach relaxation via the first excited, M J = ±5/2 doublet. The results demonstrate that dopant sites within solid-state host lattices could offer a viable alternative to rare-earth bulk magnets and high-performance SIMs, where the host matrix can be tailored to impose high symmetry and control lattice induced relaxation effects.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impact of sodium vanadium oxide (NaV 3 O 8 , NVO) material synthesis conditions on charge storage mechanism in Zn-ion aqueous batteries

The electrochemical charge storage of sodium vanadate (NaV 3 O 8 or NVO) cathodes in aqueous Zn-ion batteries has been hypothesized to be influenced by the inclusion of structural water for facilitating ion transfer in the material. Materials properties considered important (morphology, crystallite and particle size, surface area) are systematically studied herein through investigation of two NVO materials, NaV 3 O 8 ·0.34H 2 O [NVO(300)] and NaV 3 O 8 ·0.05H 2 O [NVO(500)], with different water content, acicular morphologies with different size and surface area achieved via post-synthesis heat treatment. The electrochemistry of the two materials was evaluated in aqueous Zn-ion cells with 2 M ZnSO 4 electrolyte using cyclic voltammetry, galvanostatic cycling, and rate capability testing. Furthermore, the thinner NVO(300) nanobelts (0.13 μm) demonstrate greater specific capacities and higher effective diffusion coefficients relative to the thicker NVO(500) nanorods. Notably however, while cells containing NVO(500) deliver lower specific capacity, they demonstrate enhanced capacity retention with cycling. The structural changes accompanying oxidation and reduction are elucidated via ex situ X-ray diffraction, transmission electron microscopy, and operando V K-edge X-ray absorption spectroscopy (XAS), where NVO material properties are shown to influence the ion insertion. Operando XAS verified that electron transfer corresponds directly to change in vanadium oxidation state, affirming vanadium redox as the governing electrochemical process.

25 ENERGY STORAGE↗

On the effect of metal loading on the reducibility and redox chemistry of ceria supported Pd catalysts

The effect of Pd loading on the redox characteristics of a ceria support was examined using in situ Pd K-edge XAS, Ce L 3 -edge XAS and in situ X-ray diffraction techniques. Analysis of the data obtained from these techniques indicates that the onset temperature for the partial reduction of Ce(IV) to Ce(III), by exposure to H 2 , varies inversely with the loading of Pd. Whilst the onset and completion temperatures of the reduction of Ce(IV) to Ce(III) are different, both samples yield the same maximal fraction of Ce(III) formation independent of Pd loading. Furthermore, the partial reduction of Ce is found to be concurrent with the reduction of PdO and demonstrated that the presence of metallic Pd is necessary for the reduction of the CeO 2 support. Upon passivation by room temperature oxidation, a full oxidation of the reduced ceria support was observed. However, only a mild surface oxidation of Pd was identified. The mild passivation of the Pd is found to lead to a highly reactive sample upon a second reduction by H 2 . The onset of the reduction of Pd and Ce has been demonstrated to be independent of the Pd loading after a mild passivation with both samples exhibiting near room temperature reduction in the presence of H 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deciphering helix assembly in the heliconical nematic phase via tender resonant X-ray scattering

Being a link between a uniaxial nematic and a chiral nematic, the twist bend nematic (N TB ) has been an intriguing topic for research over the last decade as a key to understanding chirality generation. Accurate description and understanding of resonance effects in helical structures provide crucial knowledge on the phase behavior beyond positional ordering. We examined the manifestation of resonance effects in N TB via tender resonant X-ray scattering (TReXS) at the sulfur K-edge. For the first time we demonstrate quantitatively that the energy dependence of the scattering peak in the N TB phase follows the energy dependence of the complex refractive indices measured by X-ray absorption. Furthermore, taking advantage of molecular energy calculation, we decipher the distinct helical pitch variation trend for symmetric/asymmetric dimers from the perspective of hybridization and reveal the strong effect of substituting oxygen for sulfur atoms on the helical pitch and the thermal helix extension.

36 MATERIALS SCIENCE↗

Band gap and electronic structure of defects in the ternary nitride BP 3 N 6 : experiment and theory

Recent advances in methods to access nitride systems by a high-pressure high-temperature approach have made possible the one-step synthesis of mixed ternary non-metal nitrides. As a prerequisite to use in a practical device, it is important to understand important bulk electronic properties, such as the band gap, as well as characterizing the presence and effect of defects that are present. In this work, the novel ternary nitride BP 3 N 6 is studied using techniques sensitive to the partial electronic density of states, specifically X-ray absorption spectroscopy and X-ray emission spectroscopy. Complementary full-potential all-electron density functional theory (DFT) calculations allow important bulk electronic parameters, such as the band gap, to be elucidated. The band gap of BP 3 N 6 has been determined to be 3.9 ± 0.2 eV and 4.1 ± 0.4 eV at the B K- and N K-edges, respectively. This is close to a theoretical value of 4.3 eV predicted by the PBEsol exchange–correlation functional and considerably less than a value of 5.8 eV predicted by the modified Becke–Johnson exchange–correlation functional. X-Ray excited optical luminescence (XEOL) measurements are performed to interrogate the presence of point defects in this system. Together with DFT calculations, these measurements reveal the presence of nitrogen vacancies which lead to multiple mid-gap trap states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis of Pt 3 Zn 1 and Pt 1 Zn 1 intermetallic nanocatalysts for dehydrogenation of ethane

Pt 3 Zn 1 and Pt 1 Zn 1 intermetallic nanoparticles supported on SiO 2 were synthesized by combining atomic layer deposition (ALD) of ZnO, incipient wetness impregnation (IWI) of Pt, and appropriate hydrogen reduction. Here, the formation of Pt 1 Zn 1 and Pt 3 Zn 1 intermetallic nanoparticles was observed by both X-ray diffraction (XRD) and synchrotron X-ray absorption spectroscopy (XAS). STEM images showed that the 2–3 nm Pt-based intermetallic nanoparticles were uniformly dispersed on a SiO 2 support. The relationships between Pt–Zn intermetallic phases and synthesis conditions were established. In situ XAS measurements at Pt L 3 and Zn K edges during hydrogen reduction provided a detailed image of surface species evolution. Owing to a combined electronic and geometric effect, Pt 1 Zn 1 exhibited much higher reactivity and stability than Pt 3 Zn 1 and Pt in both the direct dehydrogenation and oxidative dehydrogenation of ethane to ethylene reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗