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Kisslinger, Kim

Publications and source records attributed to Kisslinger, Kim.

At least 19 records

Oxide nucleation via threshold-driven volume instability in Ni oxidation

Oxide nucleation dictates the onset of metal oxidation, yet the atomistic pathways bridging initial oxygen adsorption to bulk phase transformation remain elusive. Here, we utilize in-situ atomic-resolution imaging to directly capture the nucleation of nickel oxide, revealing a threshold-driven, cooperative transformation of Ni into NiO. Our observations identify a distinct incubation period during which oxygen progressively accumulates in subsurface layers. Once a critical concentration and penetration depth are reached, a collective lattice reconfiguration is triggered, abruptly converting multiple Ni layers into NiO. Atomistic simulations corroborate this mechanism, identifying a cooperative lattice instability induced by subsurface oxygen saturation. These results establish subsurface oxygen incorporation as the missing mechanistic link between surface adsorption and three-dimensional oxide formation, providing an atomistic framework to understand and control reactive phase transformations in materials synthesis, catalysis, and degradation.

36 MATERIALS SCIENCE↗

Elucidating the Discharge Behavior of Aqueous Zinc Sulfur Batteries in the Presence of Molybdenum(IV) Chalcogenide Catalyst: The Criticality of Interfacial Electrochemistry

The aqueous zinc-sulfur battery holds promise for significant capacity and energy density with low cost and safe operation based on environmentally benign materials. However, it suffers from the sluggish kinetics of the conversion reaction. Here, we highlight the efficacy of molybdenum(IV) sulfide (MoS 2 ) to reduce the overpotential of S-ZnS conversion in aqueous electrolytes and study the discharge products formed at the solid-solid and solid-liquid interfaces using experimental and theoretical approaches. Specifically, the MoS 2 -catalyzed electrochemical conversion reaction is characterized via ex situ X-ray diffraction (XRD), transmission electron microscopy (TEM) with energy dispersive spectroscopy (EDS), Raman spectroscopy, synchrotron-based Mo K-edge X-ray absorption spectroscopy (XAS), and in situ synchrotron-based X-ray computed tomography (XCT). Additionally, operando synchrotron-based S K-edge XAS and X-ray fluorescence (XRF) maps are collected to determine the spatial evolution of sulfur-based species at the electrode-electrolyte interface. Further, coupling the operando S K-edge XAS data with the simulated spectra and fitting the data suggested a possible ZnS 2 intermediate phase.

25 ENERGY STORAGE↗

Template-Assisted Growth of High-Quality α-Phase FAPbI 3 Crystals in Perovskite Solar Cells Using Thiol-Functionalized MoS 2 Nanosheets

Formamidinium lead iodide (FAPI) has gained attention for hybrid perovskite solar cell (PSC) applications due to its enhanced stability and narrow bandgap. However, a significant challenge remains in inducing and stabilizing the elusive perovskite “black phase”—photoactive cubic α-FAPI—as the relatively bulky FA + cations tend to favor the thermodynamically stable nonphotoactive “yellow phase”. Here, in this study, we present a templated growth strategy employing thiol-functionalized MoS 2 nanosheets as templates. By introduction of 3-mercaptopropionic acid (MPA)-functionalized MoS 2 as a growth template, precise control over crystal formation was achieved, favoring the growth of high-quality α-FAPI films. These advanced templated films exhibited substantial improvements in charge transport properties, efficient light absorption, and enhanced charge extraction. As a result, the PSCs achieved a significantly enhanced power conversion efficiency (PCE) compared to the nontemplated control device, increasing from 20.6 to 22.5%. The MoS 2 -incorporated device also demonstrated excellent shelf stability, maintaining 91% of the initial PCE even after 1600 h of storage without device encapsulation.

36 MATERIALS SCIENCE↗

Synthesis and electrical transport properties of superconducting platinum silicide thin films and devices

Here, we evaluate the material characteristics of superconducting platinum silicide (PtSi) thin films as candidate materials for superconducting quantum information devices compatible with silicon technology. These films were synthesized using magnetron sputtering under ultrahigh vacuum conditions, followed by rapid thermal annealing. Polycrystalline PtSi films synthesized by this method have the favorable properties of superconducting critical temperature of 0.95 K and relatively long zero-temperature Ginzburg-Landau coherence length of 76 nm. We further studied coplanar microbridge devices fabricated by electron beam lithography and chlorine-free reactive ion etching, finding that the temperature-dependent critical current density follows the Ginzburg Landau depairing mechanism.

36 MATERIALS SCIENCE↗

Comparative S/TEM study of superconducting Ta quantum resonators by wet and dry etching types

Superconducting resonators play a pivotal role in various quantum technology applications, such as quantum computing and high-frequency communication systems. The performance of these resonators is closely tied to the properties of the superconducting films used in their fabrication. Here, in this study, we investigated the impact of wet and dry etching on tantalum (Ta) films leveraging advanced scanning transmission electron microscopy-based characterization methods and examined the morphological, chemical, and strain changes caused by the etching processes. Consequently, we report the significant differences between the two etching methods, with dry etching resulting in straight slanted sidewalls and a thinner oxidized layer, while wet etching produced curved sidewalls and undercuts. Both methods led to the formation of a residual Ta wedge at the lower part of the sidewall, causing lattice deformation, which could adversely influence the homogeneous operations of superconducting devices. These insights enhance our understanding of how etching influences superconducting films, offering valuable guidance for optimizing resonators and related devices. Our findings mark a significant stride in advancing quantum technologies and high-frequency communication by enhancing our practical understanding of superconducting material fabrication.

36 MATERIALS SCIENCE↗

Breaking Barriers in Chalcogenide Perovskite Synthesis: A Generalized Framework for Fabrication of BaMS 3 (M═Ti, Zr, Hf) Materials

Abstract Chalcogenide perovskites have garnered increasing attention as stable, non‐toxic alternatives to lead halide perovskites. However, their conventional synthesis at high temperatures (>1000 °C) has hindered widespread adoption. Recent studies have developed low‐to‐moderate temperature synthesis methods (<600 °C) using reactive precursors, yet a comprehensive understanding of the pivotal factors affecting reproducibility and repeatability remains elusive. This study delineates the critical factors in the low‐temperature synthesis of BaMS 3 (M═Zr, Hf, Ti) compounds and presents a generalized framework. Innovative approaches are developed for synthesizing BaMS 3 compounds using this framework involving organometallics for solution deposition. The molecular precursor routes, employing metal acetylacetonates to generate soluble metal–sulfur bonded complexes and metal–organic compounds to produce soluble metal‐thiolate, metal‐isothiocyanate, and metal‐trithiocarbonate species, are demonstrated to yield carbon‐free BaMS 3 . These methods have achieved the most contiguous films of BaZrS 3 and BaHfS 3 using solution deposition to date. Furthermore, a hybrid solution processing method involving stacking sputter‐deposited Zr and solution‐deposited BaS layers is employed to synthesize a contiguous, oxygen‐free BaZrS 3 film. The diffuse reflectance measurements indicate a direct bandgap of ≈ 1.85 eV for the BaZrS 3 films and ≈ 2.1 eV for the BaHfS 3 film under investigation.

25 ENERGY STORAGE↗

Characterizing Defects Inside Hexagonal Boron Nitride Using Random Telegraph Signals in van der Waals 2D Transistors

Single-crystal hexagonal boron nitride (hBN) is used extensively in many two-dimensional electronic and quantum devices, where defects significantly impact performance. Therefore, characterizing and engineering hBN defects are crucial for advancing these technologies. Here, we examine the capture and emission dynamics of defects in hBN by utilizing low-frequency noise (LFN) spectroscopy in hBN-encapsulated and graphene-contacted MoS 2 field-effect transistors (FETs). The low disorder of this heterostructure allows the detection of random telegraph signals (RTS) in large device dimensions of 100 μm 2 at cryogenic temperatures. Analysis of gate bias- and temperature-dependent LFN data indicate that RTS originates from a single trap species within hBN. By performing multi-space density functional theory (MS-DFT) calculations on a gated defective hBN/MoS 2 heterostructure model, we assign substitutional carbon atoms in boron sites as the atomistic origin of RTS. This study demonstrates the utility of LFN spectroscopy combined with MS-DFT analysis on a low-disorder all-vdW FET as a powerful means for characterizing the atomistic defects in single-crystal hBN.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Single Crystalline GeSe Van Der Waals Ribbons With Uniform Layer Stacking, High Carrier Mobility, and Adjustable Edge Morphology

Abstract Performance of the group IV monochalcogenide GeSe in solar cells, electronic, and optoelectronic devices is expected to improve when high‐quality single crystalline material is used rather than polycrystalline films. Crystalline flakes represent an attractive alternative to bulk single crystals as their synthesis may be developed to be scalable, faster, and with higher overall yield. However, large – and especially large and thin – single crystal flakes are notoriously hard to synthesize. Here it is demonstrated that vapor‐liquid‐solid growth combined with direct lateral vapor‐solid incorporation produces high‐quality single crystalline GeSe ribbons with tens of micrometers size and controllable thickness. Electron microscopy shows that the ribbons exhibit perfect equilibrium (AB) van der Waals stacking order without extended defects across the entire thickness, in contrast to the conventional case of substrate‐supported flakes where material is added via layer‐by‐layer nucleation and growth on the basal plane. Electrical measurements show anisotropic transport and a high Hall mobility of 85 cm 2 V −1 s −1 , on par with the best single crystals to date. Growth from mixed GeSe and SnSe vapors, finally, yields ribbons with unchanged structure and composition but with jagged edges, promising for applications that rely on ample chemically active edge sites, such as catalysis or photocatalysis.

99 GENERAL AND MISCELLANEOUS↗

Surface Electronic Structure of Cr Doped Bi 2 Se 3 Single Crystals

Here, by using angle-resolved photoemission spectroscopy, we showed that Bi 2-x Cr x Se 3 single crystals have a distinctly well-defined band structure with a large bulk band gap and undistorted topological surface states. These spectral features are unlike their thin film forms in which a large nonmagnetic gap with a distorted band structure was reported. We further provide laser-based high resolution photoemission data which reveal a Dirac point gap even in the pristine sample. The gap becomes more pronounced with Cr doping into the bulk of Bi 2 Se 3 . These observations show that the Dirac point can be modified by the magnetic impurities as well as the light source.

36 MATERIALS SCIENCE↗

Evolution of the Fermi Surface of 1T-VSe 2 across a Structural Phase Transition

Periodic lattice distortion, known as the charge density wave, is generally attributed to electron–phonon coupling. This correlation is expected to induce a pseudogap at the Fermi level in order to gain the required energy for stable lattice distortion. The transition metal dichalcogenide 1T-VSe 2 also undergoes such a transition at 110 K. Here, we present detailed angle-resolved photoemission spectroscopy experiments to investigate the electronic structure in 1T-VSe 2 across the structural transition. Previously reported warping of the electronic structure and the energy shift of a secondary peak near the Fermi level as the origin of the charge density wave phase are shown to be temperature independent and hence cannot be attributed to the structural transition. Our work reveals new states that were not resolved in previous studies. Earlier results can be explained by the different dispersion natures of these states and temperature-induced broadening. Only the overall size of the Fermi surface is found to change across the structural transition. These observations, quite different from the charge density wave scenario commonly considered for 1T-VSe 2 and other transition metal dichalcogenides, bring fresh perspectives toward correctly describing structural transitions. Therefore, these new results can be applied to material families in which the origin of the structural transition has not been resolved.

36 MATERIALS SCIENCE↗

Effects of residual oxygen on superconducting niobium films

The integration of niobium (Nb) into emerging superconducting circuits can enhance their performance and function. However, growth of high purity Nb can be challenging due to its high reactivity with oxygen. Here, in this study, we examine the role of residual oxygen inside the growth chamber in transforming the structural, chemical, and superconducting properties of Nb films. We demonstrate that an increase in unintentional oxygen impurities lowers the superconducting critical temperature of Nb. This evolution coincides with the reduction of Nb crystal domains, which are separated by highly disordered oxygen-rich regions. Moreover, chemical analysis reveals the formation of niobium monoxide within the film during growth. These findings provide a comprehensive picture of how residual oxygen in the growth chamber can affect the properties of the Nb films. This study contributes to the materials science and engineering knowledge of superconducting Nb growth.

36 MATERIALS SCIENCE↗

Influence of support on Rh-Co bimetallic catalysts for ethylene hydroformylation

Bimetallic Rh- and Co-based catalysts are promising materials for the heterogenous ethylene hydroformylation reaction. Here, in this study, the influence of a mesoporous silica (SBA-15) support on Rh and Co bimetallic interactions was investigated through a comparison with silica gel and alumina supports. The bimetallic catalyst supported on mesoporous silica (RhCo 3 /SBA-15) showed the best C 3 oxygenate yield among the three bimetallic catalysts. In-situ vibrational studies suggested moderate binding of the gem-dicarbonyl and Rh(CO)(C 2 H 4 ) intermediates due to this bimetallic interaction that led to improved hydroformylation performance. Kinetic studies revealed a lower hydroformylation barrier for the bimetallic compared to a Rh monometallic catalyst, and in-situ X-ray absorption spectroscopy investigations showed clear Rh-Co alloy formation on RhCo 3 /SBA-15. The bimetallic enhancement effect from the interaction with the mesoporous silica support shown here can be further optimized to design olefin hydroformylation catalysts.

58 GEOSCIENCES↗

Optimizing pulsed laser deposition of crystalline BiVO 4 thin films on yttrium-stabilized zirconia (110) substrates

Here, different conditions are explored to understand their effects on the pulsed laser deposition of BiVO 4 water splitting photoanodes, over YSZ (110) substrates. A two-step deposition (TSD) method can independently tune nucleation and bulk film growth, leading to the formation of a phase pure, crystalline BiVO 4 film with optimized water splitting activities.

36 MATERIALS SCIENCE↗

Comparison of the Effect of 2 at. % Additions of Nb and Ta on the 1100 °C Oxidation Behavior of Ni-6Al-(4,6,8) Cr Model Alloys

To continue improving alloy performance in harsh service environments, the development of alumina-forming nickel-based superalloys is essential. Current generations of these alloys heavily rely on the addition of refractory elements to enhance their mechanical properties at high temperatures; however, a systematic understanding of how such additions affect the overall oxidation behavior is still not well established, particularly from the standpoint of predicting the transition from internal to external alumina formation. The present work seeks to better understand the intrinsic effects that common minor additions of Ta and Nb have on the oxidation behavior of alumina-scale-forming γ-Ni model alloys. By combining a novel simulation approach with high-temperature oxidation experiments and advanced characterization techniques, the present study provides insightful details on the differing effects that 2 at. % addition of Ta and Nb have on the alumina scale formation of Ni-based alloys during 1100 °C oxidation.

Rodriguez, Rafael↗