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At least 433 records · Page 24

Size dependent microbial oxidation and reduction of magnetite nano- and micro-particles

The ability for magnetite to act as a recyclable electron donor and acceptor for Fe- metabolizing bacteria has recently been shown. However, it remains poorly understood whether microbe-mineral interfacial electron transfer processes are limited by the redox capacity of the magnetite surface or that of whole particles. Here we examine this issue for the phototrophic Fe(II)-oxidizing bacteria Rhodopseudomonas palustris TIE-1 and the Fe(III)-reducing bacteria Geobacter sulfurreducens, comparing magnetite nanoparticles (d ≈ 12 nm) against microparticles (d ≈ 100-200 nm). By integrating surface-sensitive and bulk-sensitive measurement techniques we observed a particle surface that was enriched in Fe(II) with respect to a more oxidized core. This enables microbial Fe(II) oxidation to occur relatively easily at the surface of the mineral suggesting that the electron transfer is dependent upon particle size. However, microbial Fe(III) reduction proceeds via conduction of electrons into the particle interior, i.e. it can be considered as more of a bulk electron transfer process that is independent of particle size. The finding has potential implications on the ability of magnetite to be used for long range electron transport in soils and sediments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

AMORE-Isoprene v1.0: a new reduced mechanism for gas-phase isoprene oxidation

Abstract. Gas-phase oxidation of isoprene by ozone (O3) and the hydroxyl (OH) and nitrate (NO3) radicals significantly impacts tropospheric oxidant levels and secondary organic aerosol formation. The most comprehensive and up-to-date chemical mechanism for isoprene oxidation consists of several hundred species and over 800 reactions. Therefore, the computational expense of including the entire mechanism in large-scale atmospheric chemical transport models is usually prohibitive, and most models employ reduced isoprene mechanisms ranging in size from ∼ 10 to ∼ 200 species. We have developed a new reduced isoprene oxidation mechanism using a directed-graph path-based automated model reduction approach, with minimal manual adjustment of the output mechanism. The approach takes as inputs a full isoprene oxidation mechanism, the environmental parameter space, and a list of priority species which are protected from elimination during the reduction process. Our reduced mechanism, AMORE-Isoprene (where AMORE stands for Automated Model Reduction), consists of 12 species which are unique to the isoprene mechanism as well as 22 reactions. We demonstrate its performance in a box model in comparison with experimental data from the literature and other current isoprene oxidation mechanisms. AMORE-Isoprene's performance with respect to predicting the time evolution of isoprene oxidation products, including isoprene epoxydiols (IEPOX) and formaldehyde, is favorable compared with other similarly sized mechanisms. When AMORE-Isoprene is included in the Community Regional Atmospheric Chemistry Multiphase Mechanism 1.0 (CRACMM1AMORE) in the Community Multiscale Air Quality Model (CMAQ, v5.3.3), O3 and formaldehyde agreement with Environmental Protection Agency (EPA) Air Quality System observations is improved. O3 bias is reduced by 3.4 ppb under daytime conditions for O3 concentrations over 50 ppb. Formaldehyde bias is reduced by 0.26 ppb on average for all formaldehyde measurements compared with the base CRACMM1. There was no significant change in computation time between CRACMM1AMORE and the base CRACMM. AMORE-Isoprene shows a 35 % improvement in agreement between simulated IEPOX concentrations and chamber data over the base CRACMM1 mechanism when compared in the Framework for 0-D Atmospheric Modeling (F0AM) box model framework. This work demonstrates a new highly reduced isoprene mechanism and shows the potential value of automated model reduction for complex reaction systems.

58 GEOSCIENCES↗

AMORE-Isoprene v1.0: A New Reduced Mechanism for Gas-Phase Isoprene Oxidation

Gas-phase oxidation of isoprene by ozone (O 3 ) and the hydroxyl (OH) and nitrate (NO 3 ) radicals significantly impacts tropospheric oxidant levels and secondary organic aerosol formation. The most comprehensive and up-to-date chemical mechanism for isoprene oxidation consists of several hundred species and over 800 reactions. Therefore, the computational expense of including the entire mechanism in large-scale atmospheric chemical transport models is usually prohibitive, and most models employ reduced isoprene mechanisms ranging in size from ∼ 10 to ∼ 200 species. We have developed a new reduced isoprene oxidation mechanism using a directed-graph path-based automated model reduction approach, with minimal manual adjustment of the output mechanism. The approach takes as inputs a full isoprene oxidation mechanism, the environmental parameter space, and a list of priority species which are protected from elimination during the reduction process. Our reduced mechanism, AMORE-Isoprene (where AMORE stands for Automated Model Reduction), consists of 12 species which are unique to the isoprene mechanism as well as 22 reactions. We demonstrate its performance in a box model in comparison with experimental data from the literature and other current isoprene oxidation mechanisms. AMORE-Isoprene's performance with respect to predicting the time evolution of isoprene oxidation products, including isoprene epoxydiols (IEPOX) and formaldehyde, is favorable compared with other similarly sized mechanisms. When AMORE-Isoprene is included in the Community Regional Atmospheric Chemistry Multiphase Mechanism 1.0 (CRACMM1AMORE) in the Community Multiscale Air Quality Model (CMAQ, v5.3.3), O 3 and formaldehyde agreement with Environmental Protection Agency (EPA) Air Quality System observations is improved. O 3 bias is reduced by 3.4 ppb under daytime conditions for O 3 concentrations over 50 ppb. Formaldehyde bias is reduced by 0.26 ppb on average for all formaldehyde measurements compared with the base CRACMM1. There was no significant change in computation time between CRACMM1AMORE and the base CRACMM. AMORE-Isoprene shows a 35 % improvement in agreement between simulated IEPOX concentrations and chamber data over the base CRACMM1 mechanism when compared in the Framework for 0-D Atmospheric Modeling (F0AM) box model framework. This work demonstrates a new highly reduced isoprene mechanism and shows the potential value of automated model reduction for complex reaction systems.

Automated Model Reduction↗

In Situ TEM Study of the Amorphous-to-Crystalline Transition during Dielectric Breakdown in TiO 2 Film

Dielectric breakdown of oxides is a main limiting factor for improvement of the performance of electronic devices. Present understanding suggests that defects produced by intense voltage accumulate in the oxide to form a percolation path connecting the two electrodes and trigger the dielectric breakdown. However, reports on directly visualizing the process at nanoscale are very limited. Here, we apply in situ transmission electron microscopy to characterize the structural and compositional changes of amorphous TiO 2 under extreme electric field (~100 kV/mm) in a Si/TiO 2 /W system. Upon applying voltage pulses, the amorphous TiO 2 gradually transformed to crystalline sub-stoichiometric rutile TiO 2-x and the Magnéli phase Ti 3 O 5 . The transitions started fromat the anode/oxide interface under both field polarities. Preferred growth orientation Epitaxial growth of rutile TiO 2-x with respect toon the Si substrate was observed when Si was the anode, while oxidation and melting of the W probe occurred when W was the anode. We associate the TiO 2 crystallization process with the electrochemical reduction of TiO 2 , polarity-dependent oxygen migration, and Joule heating. The experimental results are supported by our phase-field modeling. These findings provide direct details of the defect formation process during dielectric breakdown in amorphous oxides and will help the design of electronic devices with higher efficiency and reliability.

36 MATERIALS SCIENCE↗

Role of Metal Cocatalysts in the Photocatalytic Production of Hydrogen from Water Revisited

The use of photocatalysts to promote the production of molecular hydrogen from water, following the so-called water splitting reaction, continues to be a promising route for the green production of fuels. The molecular basis of this photocatalysis is the photoexcitation of electrons from the valence band of semiconductors to their conduction band, from which they can be transferred to chemical reactants, protons in the case of water, to promote a reduction reaction. The mechanism by which such a process takes place has been studied extensively using titanium oxide, a simple material that fulfills most requirements for water splitting. However, photocatalysis with TiO 2 tends to be highly inefficient; a cocatalyst, commonly a late transition metal (Au, Pt) in nanoparticle form, needs to be added to facilitate the production of H 2 . The metal is widely believed to help with the scavenging of the excited electrons from the conduction band of the semiconductor in order to prevent their recombination with the accompanying hole formed in the valence band, a step that cancels the initial photon absorption and competes with the photolytic chemical reduction. Here we review and analyze the molecular basis for that mechanism and argue for an alternative explanation, that the role of the metal is to help with the recombination of the atomic hydrogen atoms produced by proton reduction on the semiconductor surface instead. First, we summarize what is known about the electronic structure of these photocatalysts and how the electronic levels need to line up for the reduction of protons in water to be feasible. Next, we review the current understanding of the dynamics of the steps associated with the absorption of photons, the de-excitation via electron–hole pair recombination and fluorescence decay, and the electronic transitions that lead to proton reduction, and contrast those with the rates of the chemical steps required to produce molecular hydrogen. The following section addresses the changes introduced by the addition of the metal cocatalyst, comparatively evaluating its role as either an electron scavenger or a promoter of the recombination of hydrogen atoms. A discussion of the viable chemical mechanisms for the latter pathway is included. Finally, we briefly mention other associated aspects of this photocatalysis, including the possible promotion of H 2 production with visible light via resonant excitation of the surface plasmon of Au nanoparticles, the use of single-metal (Au, Pt) atom catalysts and of yolk–shell nanostructures, and the reduction of organic molecules. We end with a brief personal perspective on the possible generality of the concepts introduced in this Critical Review.

08 HYDROGEN↗

The short-term reduction of uranium by nanoscale zero-valent iron (nZVI): role of oxide shell, reduction mechanism and the formation of U( v )-carbonate phases

Nanoscale zero-valent iron (nZVI) is a potential remediation agent for uranium-contaminated groundwaters, however, a complete mechanistic understanding of the processes that lead to uranium immobilization has yet to be achieved. In this study, the short-term anoxic reaction of U(VI) with fresh, (anoxic) aged and corroded nZVI particles was investigated under aqueous conditions conducive to the formation of thermodynamically stable U(VI)-Ca-CO3 ternary aqueous complexes. The first stage of the reaction between U(VI) and nZVI was assigned to sorption processes with the formation of surface U(VI)-carbonate complexes. Aged nZVI removed U(VI) faster than either fresh or corroded nZVI and it is hypothesized that U reduction initially occurs through the transfer of one electron from Fe(II) in the nZVI surface oxide layer. Evidence for reduction to U(V) was obtained through X-ray photoelectron spectroscopy and by determination of U-O bond distances of ~2.05 Å and 2.27 Å by U LIII-edge X-ray absorption spectroscopy detection of U-O bond distances at ~2.05 Å and 2.27 Å with these distances , similar to thoseat observed for the U(V) site in the mixed U(V)/U(VI) carbonate mineral wyartite. Scanning transmission electron microscopy also demonstrated that U was present as a nanoparticulate phase after one day of reaction, rather than a surface complex. Further reduction to U(IV), as observed in previous studies, would appear to be rate-limiting and coincident with the transformation of this meta-stable U-carbonate phase to uraninite (UO2).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Waste Minimization of HyBRID Decontamination Process - 17060

The Korea Atomic Energy Research Institute (KAERI) developed a Hydrazine base reductive metal ion decontamination (HyBRID) and related pre-oxidation techniques for use in decommissioning a nuclear facility. Inorganic chemicals were used to increase the integrity of the radioactive waste in a repository. Decomposition and precipitation of residual reagents with inorganic chemicals were introduced to minimize the final waste volume. The waste volume was calculated theoretically and demonstrated in a small-scale waste treatment system and bench-scale candle filtration system. The total waste volume of the HyBRID process was less than 1/10 of that of commercial processes, and spent ion-exchange resins were significantly reduced to 5% of that of commercial processes. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Sequential oxidation-depolymerization strategies for lignin conversion to low molecular weight aromatic chemicals

Lignin is the largest source of bio-derived aromatic chemicals, and oxidative conversion of this polymeric material can generate valuable oxygenated aromatic compounds. Oxidative depolymerization of lignosulfonate feedstocks under alkaline conditions is used commercially for vanillin production. Recent studies have led to other oxidation methods that access different aromatic products from lignin in good yields. A particularly effective strategy that accesses some of the highest yields of aromatic monomers to date features a two-step process in which the oxidation of specific alcohol groups in lignin is followed by an oxidative, reductive, or redoxneutral step that cleaves the polymer into aromatic monomers and oligomers. Studies of model compounds have provided crucial mechanistic insights and contributed to the development of effective lignin depolymerization methods. Furthermore, this review provides a general overview of lignin depolymerization methods, followed by a survey of oxidation-depolymerization methods that access oxygenated aromatic monomers in good yields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Insights into the methanol synthesis mechanism via CO 2 hydrogenation over Cu-ZnO-ZrO2 catalysts: Effects of surfactant/Cu-Zn-Zr molar ratio

In this study, we evaluated aspects of the CO 2 hydrogenation mechanism, correlating structure-activity relationships of Cu-ZnO-ZrO 2 catalysts prepared by one-pot surfactant-assisted co-precipitation with different surfactant ratios. Identifying the CO 2 hydrogenation pathway intermediates is key to controlling the reaction selectivity. Experimental evidence shows that the CO 2 is dissociating into CO* and O* onto the surface of the Cu-ZnO-ZrO 2 catalyst. The adsorption and dissociation of CO2 were evidenced by a combination of in situ ambient-pressure X-ray Photoelectron Spectroscopy (AP-XPS) and Fourier Transform Infrared Spectroscopy (FTIR) with a transmission cell. AP-XPS showed that the catalysts are composed of a Cu 2+ , Zr 3+ , and Zr 4+ mixture and two kinds of Zn 2+ species. After the H 2 reduction process, only Cu 2+ was reduced to Cu0. The Zn and Zr species were oxidized by the dissociated O* species. In situ transmission FTIR showed that CO was adsorbed onto the Cu+/0 sites. The catalyst with the higher surfactant molar ratio exhibited the highest CO 2 conversion close to the equilibrium conversion, as well as a good methanol formation rate.

36 MATERIALS SCIENCE↗

Polar algae flaunt their zinc assets

Metal ions have been at the centre of pivotal points in the evolution of extant life. Oxygen-evolving photosynthesis, which irrevocably reshaped the geochemistry and biology of our planet, has an absolute requirement for metal ions to harvest light, split water and transfer electrons. Access to abundant oxygen then led to the propagation of organisms capable of oxidative metabolism, a process that is also dependent on metal ions for electron transfer and reduction of molecular oxygen. Because of the essential links between metal ions and the proteins that require them to function, as well as changes in metal bioavailability through time, metals have shaped the trajectories that evolution can take. Iron typically steals this show, but with access to whole-genome sequences and transcriptomes, the imprint that zinc has made on biology is coming into focus. Writing in Nature Ecology & Evolution, Ye and colleagues present new insights into the complex connections between zinc bioavailability, adaptation of algae to the polar oceans and the evolution of regulatory networks. By combining field and laboratory-based analyses, the authors suggest that expanded families of zinc-binding proteins have enabled the green alga Microglena sp. YARC to flourish in the harsh conditions of the polar Southern Ocean (Fig. 1). As the waters where this alga occurs are known for their enrichment of zinc, the authors further propose that availability of this metal ion was directly responsible for successful microalgal colonization of polar oceans. To test this hypothesis, the authors compare meta-transcriptomes collected from pole-to-pole and find positive correlations between higher copy numbers for transcripts encoding putative zinc-binding proteins, higher latitudes, lower surface temperatures and dissolved zinc.

59 BASIC BIOLOGICAL SCIENCES↗

Interfacial chemistry and valence band offset between GaN and Al{sub 2}O{sub 3} studied by X-ray photoelectron spectroscopy

The interface region between Ga-face n-type GaN and Al{sub 2}O{sub 3} dielectric (achieved via atomic-layer deposition or ALD) is investigated by X-ray photoelectron spectroscopy (XPS). An increase in the Ga-O to Ga-N bond intensity ratio following Al{sub 2}O{sub 3} deposition implies that the growth of an interfacial gallium sub-oxide (GaO{sub x}) layer occurred during the ALD process. This finding may be ascribed to GaN oxidation, which may still happen following the reduction of a thin native GaO{sub x} by trimethylaluminum (TMA) in the initial TMA-only cycles. The valence band offset between GaN and Al{sub 2}O{sub 3}, obtained using both core-level and valence band spectra, is found to vary with the thickness of the deposited Al{sub 2}O{sub 3}. This observation may be explained by an upward energy band bending at the GaN surface (due to the spontaneous polarization induced negative bound charge on the Ga-face GaN) and the intrinsic limitation of the XPS method for band offset determination.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Atomic-scale polarization switching in wurtzite ferroelectrics

Ferroelectric wurtzites have the potential to revolutionize modern microelectronics because they are easily integrated with multiple mainstream semiconductor platforms. However, the electric fields required to reverse their polarization direction and unlock electronic and optical functions need substantial reduction for operational compatibility with complementary metal-oxide semiconductor (CMOS) electronics. To understand this process, we observed and quantified real-time polarization switching of a representative ferroelectric wurtzite (Al 0.94 B 0.06 N) at the atomic scale with scanning transmission electron microscopy. The analysis revealed a polarization reversal model in which puckered aluminum/boron nitride rings in the wurtzite basal planes gradually flatten and adopt a transient nonpolar geometry. Independent first-principles simulations reveal the details and energetics of the reversal process through an antipolar phase. Furthermore, this model and local mechanistic understanding are a critical initial step for property engineering efforts in this emerging material class.

36 MATERIALS SCIENCE↗

Structural evolution of the double perovskites Sr{sub 2}B'UO{sub 6} (B' = Mn, Fe, Co, Ni, Zn) upon reduction: Magnetic behavior of the uranium cations

Highlights: {yields} Evolution of the double perovskites Sr{sub 2}B'UO{sub 6} upon reduction were studied by XRPD. {yields} Orthorhombic (Pnma) disordered perovskites SrB'{sub 0.5-x}U{sub 0.5+x}O{sub 3} were obtained at 900 {sup o}C. {yields} U{sup 5+/4+} and Zn{sup 2+} cations are distributed at random over the octahedral positions. {yields} AFM ordering for the perovskite with B' = Zn appears below 30 K. -- Abstract: We describe the preparation of five perovskite oxides obtained upon reduction of Sr{sub 2}B'UO{sub 6} (B' = Mn, Fe, Co, Ni, Zn) with H{sub 2}/N{sub 2} (5%/95%) at 900 {sup o}C during 8 h, and their structural characterization by X-ray powder diffraction (XRPD). During the reduction process there is a partial segregation of the elemental metal when B' = Co, Ni, Fe, and the corresponding B'O oxide when B' = Mn, Zn. Whereas the parent, oxygen stoichiometric double perovskites Sr{sub 2}B'UO{sub 6} are long-range ordered concerning B' and U cations. The crystal structures of the reduced phases, SrB'{sub 0.5-x}U{sub 0.5+x}O{sub 3} with 0.37 < x < 0.27, correspond to simple, disordered perovskites; they are orthorhombic, space group Pnma (No. 62), with a full cationic disorder at the B site. Magnetic measurements performed on the phase with B' = Zn, indicate uncompensated antiferromagnetic ordering of the U{sup 5+}/U{sup 4+} sublattice below 30 K.

36 MATERIALS SCIENCE↗

Structural Transformation and Degradation of Cu Oxide Nanocatalysts during Electrochemical CO 2 Reduction

The electrochemical CO 2 reduction reaction (CO 2 RR) holds enormous potential as a carbon-neutral route to the sustainable production of fuels and platform chemicals. The durability for long-term operation is currently inadequate for commercialization, however, and the underlying deactivation process remains elusive. A fundamental understanding of the degradation mechanism of electrocatalysts, which can dictate the overall device performance, is needed. In this work, we report the structural dynamics and degradation pathway of Cu oxide nanoparticles (CuO x NPs) during the CO 2 RR by using in situ small-angle X-ray scattering (SAXS) and X-ray absorption spectroscopy (XAS). The in situ SAXS reveals a reduction in the size of NPs when subjected to a potential at which no reaction products are detected. At potentials where the CO 2 RR starts to occur, CuO x NPs are agglomerated through a particle migration and coalescence process in the early stage of the reaction, followed by Ostwald ripening (OR) as the dominant degradation mechanism for the remainder of the reaction. As the applied potential becomes more negative, the OR process becomes more dominant, and for the most negative applied potential, OR dominates for the entire reaction time. The morphological changes are linked to a gradual decrease in the formation rate for multicarbon products (C 2 H 4 and ethanol). Other reaction parameters, including reaction intermediates and local high pH, induce changes in the agglomeration process and final morphology of the CuO x NPs electrode, supported by post-mortem ex situ microscopic analysis. The in situ XAS analysis suggests that the CuO x NPs reduced into the metallic state before the structural transformation was observed. The introduction of high surface area carbon supports with ionomer coating mitigates the degree of structural transformation and detachment of the CuO x NPs electrode. These findings show the dynamic nature of Cu nanocatalysts during the CO 2 RR and can serve as a rational guideline toward a stable catalyst system under electrochemical conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Organic and Aqueous Redox Speciation of Cu(III) Periodate Oxidized Transuranium Actinides

A hexavalent group actinide separation process could streamline used nuclear fuel recycle and waste management. The limiting factor to such a process compatible with current fuel dissolution practices is obtaining and maintaining hexavalent Am, in molar nitric acid due to the high reduction potential of the Am(VI)/Am(III) couple (1.68 V vs SCE). Two strong oxidants, sodium bismuthate and Cu(III) periodate, have demonstrated quantitative oxidation of Am under molar acid conditions and better than 50% recovery by diamyl amylphosphonate (DAAP) is possible under these same conditions. This work considers the use of Cu(III) periodate to oxidize Np(V) to Np(VI) and Pu(IV) to Pu(VI) and recover these elements by extraction with DAAP. A metal:oxidant ratio of 1:1.2 and 1:3 was necessary to quantitatively oxidize Np(V) and Pu(IV), respectively, to the hexavalent state. Extraction of hexavalent Np, Pu, and Am by 1 M DAAP in n-dodecane was measured using UV-Vis [Pu(VI), Am (VI)] and NIR [Np(VI)]. Distribution values of Am(VI) were found to match previous tracer level studies. The organic phase spectra of Np, Pu, and Am are presented and molar absorptivities are calculated for characteristic peaks. Hexavalent Pu was found to be stable in the organic phase while Np(VI) showed some reduction to Np(V) and Am was present as Am(III), Am(V), and Am(VI) species in aqueous and organic phases during the extraction experiments. These results demonstrate, for the first time, the ability to recover macroscopic amounts of americium that would be present during fuel reprocessing and are the first characterization of Am organic phase oxidation state speciation relevant to a hexavalent group actinide separation process under acidic conditions.

americium↗

Effect of Carbon Deposition on the Oxidation Rate of Copper/Bentonite in the Chemical Looping Process

The presented work is part of the Industrial Carbon Management Initiative (ICMI) on the development of metal oxide oxygen carriers for use in the chemical looping combustion process. An oxygen carrier, CuO/bentonite (60:40%), was reacted with methane gas and then oxidized in air. The change in weight and reaction gas concentrations were measured using a thermogravimetric analyzer (TGA) equipped with a real-time gas analyzer. The reduction–oxidation cycle was conducted within the temperature range of 750–900 °C for 10 cycles, using 20, 50, and100% CH{sub 4} concentrations in N{sub 2} for the reduction segment and dry air for the oxidation segment. Several analysis methods were evaluated to fit the oxidation of reduced CuO (i.e., Cu) data over the complete conversion range with suitable rate expressions derived from existing models for oxidation, including the shrinking core model (diffusion and reaction control), first- and second-order reaction rates, parallel and series reaction mechanisms, and Johnson–Mehl–Avrami (JMA) rate. The best agreement between the experimental data and the models of the Cu oxidation was accomplished using the JMA model. The reactivity of the oxygen carrier during the oxidation reactions was affected by the CH{sub 4} concentration as well as the temperature. The rate of fractional uptake of oxygen onto the carrier decreased as the temperature increased, contrary to expectations and indicative that the mechanism is changing during the test. Analysis of the exit gas provided evidence of carbon deposition on the reduced sorbent particle and resulted in the CO{sub 2} product upon oxidation. The oxidation of this carbon releases significant heat that is capable of changing the particle morphology (Zhu, Y.; Mimura, K.; Isshiki, M. Oxid. Met. 2004, 62, 207-222). On the basis of experimental results, the overall reaction process in the fuel reactor may be considered to consist of the decomposition of CH{sub 4} into C and H{sub 2} and reduction of CuO/bentonite by the resulting H{sub 2} and the parallel reaction of CH{sub 4} with CuO/bentonite. The extent of carbon deposition in the carrier particle increased with an increasing temperature and CH{sub 4} concentration. This deposited carbon not only leads to CO{sub 2} release from the oxidation reactor but, more importantly, causes degredation of the carrier capacity and its reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Room Temperature Electrorefining of Rare Earth Metals from End-of-use Nd-Fe-B Magnets

Recovering rare earth elements (REE) from used permanent magnets, which contains about 30 wt.% of rare earth elements, has been persistent technological challenge. Current recycling methods relies on pyrometallurgical or hydrometallurgical processes which are energy- and chemical- intensive and not economically and environmentally viable for rare earth containing magnets. Enabling efficient and simplistic recovery and refining of REEs contained in End-of-Use (EoU) products, such as Neodymium-Iron-Boron (Nd-Fe-B) based magnets will play an important and complementary role in the total supply of REEs in the future. We designed a new electrochemical method and demonstrated a room temperature one-pot process that concurrently separates and electroplates REE from commercial Nd-Fe-B magnets. By establishing selective oxidation and reductive potential as electrochemical control parameter along with electrochemically compatible non-aqueous electrolyte system, we demonstrated selective electroleaching of lanthanides (Nd and Preseodymium (Pr)) from anode and concurrent plating as alloy at Pt cathode. The morphological and chemical evolution of the Nd-Fe-B magnets during electroleaching reveals the electrochemical stimuli and rate of dissolution depends on microstructural complexities of the Nd-Fe-B magnet. The concomitant electroplating process leads to Nd-Pr based alloy which can be used as raw metallic alloy for manufacturing new permanent magnet and other devices. Our study demonstrates a scalable separation and refining methodology, based on widely available organic electrolyte system and without any consumptive chemical use, for selective lanthanide recovery from waste magnets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗