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Mullins, C. Buddie

Publications and source records attributed to Mullins, C. Buddie.

Elucidating the mechanism underlying the augmented capacity of MoO 2 as an anode material in Li-ion batteries

Transition-metal oxide anode materials have been observed to possess an intriguing surplus of capacity beyond the expected values based on conversion reaction. However, the mechanisms behind this phenomenon have remained contentious and elusive. Here, this study focuses on synthesized nanosized molybdenum dioxide and its electrochemical performance as an anode material for Li-ion batteries. Our findings reveal a substantial increase in capacity upon cycling, achieving approximately 1688 mA h g -1 , nearly double the theoretical capacity, after 700 cycles at a 1C rate. To elucidate the mechanisms underlying this augmented capacity, a comprehensive analysis employing in situ and ex situ X-ray diffraction, X-ray absorption spectroscopy, scanning electron microscopy, and transmission electron microscopy was conducted at various stages of the Li-ion cell cycling. Our results indicate that no conversion reaction occurs during the initial discharge phase, with Li 2 O and Mo remaining undetected. Instead, Li 0.98 MoO 2 is generated upon lithiation. Further materials characterization employing electron energy loss spectroscopy and energy-dispersive X-ray spectroscopy on the cycled electrode suggests the potential formation of a metallic Li-rich layer at the interface of the Li-ion intercalated phase subsequent to the formation of Li 0.98 MoO 2 , contributing to the surplus Li storage. Moreover, electrochemical impedance spectroscopy coupled with ex situ SEM and TEM analyses reveals that alterations in particle size and morphology, along with changes in the solid electrolyte interphase (SEI) resistance, are instrumental in the capacity variation observed upon cycling.

25 ENERGY STORAGE↗

CO Dissociation on model Co/SiO 2 catalysts – effect of adsorbed hydrogen

Here we found experimental evidence that shows the effect that adsorbed hydrogen can have on CO dissociation. For cobalt nanoparticles supported on SiO 2 , adsorbed hydrogen enhances CO dissociation. In contrast, adsorbed hydrogen inhibits CO dissociation on a cobalt film supported on SiO 2 . Considering the nature of cobalt deposited by physical vapor deposition, these results can be explained by a preference for CO dissociation to follow the hydrogen-assisted dissociation mechanism on FCC cobalt and step-edges, while the direct dissociation mechanism is preferred on HCP cobalt. These results are in agreement with previous theoretical results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Blade-Type Reaction Front in Micrometer-Sized Germanium Particles during Lithiation

To investigate the lithium transport mechanism in micrometer-sized germanium (Ge) particles, in situ focused ion beam-scanning electron microscopy was used to monitor the structural evolution of individual Ge particles during lithiation. Our results show that there are two types of reaction fronts during lithiation, representing the differences of reactions on the surface and in bulk. Further, the cross-sectional SEM images and transmission electron microscopy characterizations show that the interface between amorphous Li x Ge and Ge has a wedge shape because of the higher Li transport rate on the surface of the particle. The blade-type reaction front is formed at the interface of the amorphous Li x Ge and crystalline Ge and is attributed to the large strain at the interface.

25 ENERGY STORAGE↗

Evaluation of a V 8 C 7 Anode for Oxygen Evolution in Alkaline Media: Unusual Morphological Behavior

Metallic vanadium carbide (V 8 C 7 ) with cubic symmetry is examined as an oxygen evolution reaction (OER) precatalyst in alkaline media. Herein, we used quasi in situ scanning electron microscopy and energy-dispersive X-ray spectrometry to investigate the structural transformation of the precatalyst V 8 C 7 microparticles during extended cyclic voltammetric (CV) OER testing. Interestingly, an anisotropic morphological transformation (from a distorted sphere to a cuboid) of V 8 C 7 was observed. Our theoretical and experimental results strongly suggest that this morphological change happens due to the selective self-oxidation and dissolution of the V 8 C 7 (110) and (111) surfaces and the subsequent exposure of the relatively stable (100), (010), and (001) surfaces. Lastly, these results also suggest that these stable facets are preferable for the OER, and a current density of 10 mA·cm –2 was delivered at an overpotential of 503 mV after the extended CV OER testing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Perspective on the Electrochemical Oxidation of Methane to Methanol in Membrane Electrode Assemblies

Direct conversion of methane to methanol has been a long-sought objective. Partial oxidation by thermal catalysis is possible but suffers from a rapid loss in methanol selectivity with increasing methane conversion. More recently, the electrochemical oxidation of methane, using water, rather than oxygen, as the oxidizing agent has been considered in both aqueous electrolyte systems and membrane-electrode assemblies (MEAs). While promising results have been demonstrated using MEAs, the absence of key metrics of system performance make it hard to compare and contrast the results of different investigators. Overall, this Perspective examines why MEAs are well-suited for the electrochemical oxidation of methane, defines the metrics for assessing MEA performance, and reviews the progress in the field. An analysis of the challenges to finding suitable electrocatalysts is included with the aim of guiding the search for electrocatalysts that would be both active and selective for the conversion of methane to methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hydrogen desorption from the surface and subsurface of cobalt

The influence of coverage on the diffusion of hydrogen into the subsurface of cobalt was studied using density functional theory (DFT) and temperature programmed desorption (TPD). DFT calculations show that as the hydrogen coverage on Co(0001) increases, the barrier for hydrogen diffusion into the bulk decreases by 20%. Additionally, subsurface hydrogen on a hydrogen covered surface was found to be more stable when compared to a clean cobalt surface. To test these theoretical findings experimentally, excited hydrogen was used in an ultra-high vacuum environment to access higher hydrogen coverages. Here, our TPD studies showed that at high hydrogen coverages, a sharp low temperature feature appeared, indicating the stabilization of subsurface hydrogen. Further DFT calculations indicate that this sharp low temperature feature results from associative hydrogen desorption from a hydrogen saturated surface with a population of subsurface hydrogen. Microkinetic modelling was used to model the TPD spectra for hydrogen desporption from cobalt with and without subsurface hydrogen, showing reasonable agreement with experiment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Moisture-Driven Formation and Growth of Quasi-2-D Organolead Halide Perovskite Crystallites

Ruddlesden–Popper phase quasi-2-D organolead halide perovskites like n-butylammonium methylammonium lead iodide (nBA-MAPI) exhibit improved moisture stability over typical 3-D perovskite materials, making them exciting for use in a variety of applications such as photovoltaic (PV) devices. This improved stability is the result of a unique disproportionation-based degradation mechanism that protects the bulk of the nBA-MAPI from extensive damage through the formation of a protective, low-n surface layer. In addition to this surface layer, nBA-MAPI films also exhibit the dynamic growth of micrometer-scale crystallites and cracks at the surface of the film, unique and potentially important byproducts of quasi-2-D perovskite disproportionation. Here, we present a detailed study of these crystallites using several analytical techniques including photoluminescence spectroscopy (PL), confocal fluorescence microscopy (CFM), atomic force microscopy (AFM) combined with time-of-flight-secondary ion mass spectrometry (ToF-SIMS), and others in an effort to better understand the relationship between material disproportionation and crystallite growth. Our results show that the crystallites form after exposure to humid air and confirm that they are composed of low-n phases of nBA-MAPI. The crystallites are found to extend into the interior of the film and exhibit continued growth while exposed to moisture over 72 h. This growth is accompanied by both a decrease in the bulk 2-D phase and an increase in a 3-D-like phase in the surface PL spectra, indicating that the crystallites are likely a product of moisture-driven disproportionation. Importantly, similar crystallites are also observed to form within model PV devices, indicating that such processes must be accounted for when designing future devices containing materials like nBA-MAPI.

36 MATERIALS SCIENCE↗

Cobalt Metal–Cobalt Carbide Composite Microspheres for Water Reduction Electrocatalysis

Microspheres of cobalt metal–cobalt carbide (Co–Co x C, Co x C: Co 2 C and Co 3 C) composite with carbon shells were prepared via an OH – - and Cl – -assisted polyol method and explored for electrocatalytic activity and stability for the hydrogen evolution reaction (HER) in acidic media. From our transmission electron microscopy observations, the outermost surfaces of the as-prepared Co–Co x C composites were primarily covered with Co 2 C crystallites. Our best performing electrocatalyst exhibited superior HER activity with an overpotential of 78 mV to reach a current density of -10 mA·cm –2 , a Tafel slope of 87.8 mV·dec –1 , and 1 h of electrode durability. We show that this excellent HER performance is primarily due to the superior intrinsic activity of Co 2 C, as well as the high electrical conductivity resulting from the inclusion of cobalt metal and the presence of graphitic carbon shells in and on the composite, respectively. Using both computational and experimental approaches, we determine here that the carbon-rich cobalt carbide (Co 2 C) phase is more favorable for the HER than the carbon-poor phase (Co 3 C).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Low temperature dissociation of CO on manganese promoted cobalt(poly)

We observe that metallic manganese alloyed with polycrystalline cobalt promotes the dissociation of CO. Increasing coverages of Mn on Co facillitate stronger molecular CO binding energies and stronger C(ad) + O(ad) binding energies. These findings show the role of metallic manganese in promoting model Co Fischer–Tropsch catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗