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DOE OSTI2020

Achieving high volumetric EDLC carbons via hydrothermal carbonization and cyclic activation

A novel activation method involving hydrothermal carbonization (HTC) and a pressure-induced low temperature oxidation has been demonstrated for cellulose derived HTC char by using hydrogen peroxide as an active di-oxygen source. The optimized porosity versus gravimetric capacitance results from cellulose derived HTC char synthesized at 220 °C. Almost homogeneous and small particle size micro-ellipse/sphere, relatively high surface area and narrow pore size distributions lead to a high bulk density, i.e. 0.73 g cm -3 , of coating type electrodes, which is much denser than those manufactured from steam activated carbons for supercapacitor industry, i.e., 0.52 g cm -3 . The resulting carbon prepared herein achieves a relatively high volumetric capacitance in an organic electrolyte-based supercapacitor reaching a competitive value of industrial system with the features of environment friendly, cost-effective as well as high yield, and less energy consumption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Methanobactin from methanotrophs: genetics, structure, function and potential applications

ABSTRACT Aerobic methane-oxidizing bacteria of the Alphaproteobacteria have been found to express a novel ribosomally synthesized post-translationally modified polypeptide (RiPP) termed methanobactin (MB). The primary function of MB in these microbes appears to be for copper uptake, but MB has been shown to have multiple capabilities, including oxidase, superoxide dismutase and hydrogen peroxide reductase activities, the ability to detoxify mercury species, as well as acting as an antimicrobial agent. Herein, we describe the diversity of known MBs as well as the genetics underlying MB biosynthesis. We further propose based on bioinformatics analyses that some methanotrophs may produce novel forms of MB that have yet to be characterized. We also discuss recent findings documenting that MBs play an important role in controlling copper availability to the broader microbial community, and as a result can strongly affect the activity of microbes that require copper for important enzymatic transformations, e.g. conversion of nitrous oxide to dinitrogen. Finally, we describe procedures for the detection/purification of MB, as well as potential medical and industrial applications of this intriguing RiPP.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Irradiation Effect on Noble Metal Particles in Water Using in situ Liquid Cell STEM Observation

During geologic disposal of spent nuclear fuel (SNF) in an engineered nuclear waste repository, once all other barriers have degraded, oxidizing may occur at the solid-water interface owing to a self-generated radiolytic field. The repository design includes large quantities of iron (Fe), that is anticipated to corrode under an anoxic environment, and generate hydrogen (H 2 ) gas. This H 2 gas is thought to be able to suppress the dissolution of SNF through a catalytic reaction with noble metal particles (NMP) that are pre-existing in the SNF. This interaction leads to the decomposition of the major oxidant, hydrogen peroxide (H 2 O 2 ). In conclusion, these processes are described in the Fuel Matrix Degradation (FMD) model that is being used to predict SNF degradation rates. The NMP, therefore, plays an important role within the FMD model.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Enhancement of reactive oxygen species production by ultra-short electron pulses

The development of laser-driven accelerators-on-chip has provided an opportunity to miniaturize devices for electron radiotherapy delivery. Laser-driven accelerators produce highly time-compressed electron pulses, on the 100 fs to 1 ps scale. This delivers electrons at high peak power yet low average beam current compared with conventional delivery devices, which generate pulses of approximately 3 µs. The biophysical effects of this time structure, however, are unclear. Here, we use a Monte Carlo simulation approach to explore the effects of the electron beam time structure on the production of reactive oxygen species (ROS) in water. Our results show a power law increase in the generation of hydroxyl ions per deposited electron with decreasing pulse length over the pulse length range of 10 µs to 100 fs. Similar trends were observed for hydrogen peroxide, superoxide, hydroperoxyl, hydronium and solvated electrons. In practical terms, this indicates a fourfold increase in the efficiency of free radical production for sub-picosecond pulses, relative to that of conventional microsecond pulses, for the same number of deposited electrons.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Wet-Etching of Acoustically Spalled GaAs for Substrate Reuse

Acoustic spalling is a promising technique for substrate reuse in the fabrication of gallium arsenide (GaAs) photovoltaic cells. However, the acoustic spalling process can leave the substrate with areas of rough surface morphology that can interfere with subsequent cell growth and processing. In this work, we investigate the use of wet etchants to smooth the surface of acoustically spalled GaAs substrates. We evaluated six different etchants. Of those tested, an 8:1:1 mixture of sulfuric acid, hydrogen peroxide, and water at 30 degrees C and a moderate stirring rate showed the greatest roughness reduction per mass loss while producing the desired morphology. This etchant was then applied to an acoustically spalled 2-inch GaAs wafer. A single-junction GaAs cell was then grown via metalorganic vapor-phase epitaxy on this substrate, an acoustic spalled substrate without a smoothing etch, and an epi-ready substrate. Use of the 8:1:1 H2SO4:H2O2:H2O etchant produced cells an average efficiency of 12.8% as compared to that of 2.0% grown on the unetched acoustically spalled substrate and 16.3% grown on the epi-ready substrate. The results of this work demonstrate that wet etching is a viable method for smoothing the surface of spalled GaAs substrates, paving the way for substrate reuse via acoustic spalling at efficiencies that approach growth on epi-ready substrates.

etching↗

DOE OSTI2022

Mechanistic assessment of tolerance to iron deficiency mediated by Trichoderma harzianum in soybean roots

Abstract Aims Iron (Fe) deficiency in soil is a continuing problem for soybean (Glycine max L.) production, partly as a result of continuing climate change. This study elucidates how Trichoderma harzianum strain T22 (TH) mitigates growth retardation associated with Fe-deficiency in a highly sensitive soybean cultivar. Methods and Results Soil TH supplementation led to mycelial colonization and the presence of UAOX1 gene in roots that caused substantial improvement in chlorophyll score, photosynthetic efficiency and morphological parameters, indicating a positive influence on soybean health. Although rhizosphere acidification was found to be a common feature of Fe-deficient soybean, the upregulation of Fe-reductase activity (GmFRO2) and total phenol secretion were two of the mechanisms that substantially increased the Fe availability by TH. Heat-killed TH applied to soil caused no improvement in photosynthetic attributes and Fe-reductase activity, confirming the active role of TH in mitigating Fe-deficiency. Consistent increases in tissue Fe content and increased Fe-transporter (GmIRT1, GmNRAMP2a, GmNRAMP2b and GmNRAMP7) mRNA levels in roots following TH supplementation were observed only under Fe-deprivation. Root cell death, electrolyte leakage, superoxide (O2•–) and hydrogen peroxide (H2O2) substantially declined due to TH in Fe-deprived plants. Further, the elevation of citrate and malate concentration along with the expression of citrate synthase (GmCs) and malate synthase (GmMs) caused by TH suggest improved chelation of Fe in Fe-deficient plants. Results also suggest that TH has a role in triggering antioxidant defence by increasing the activity of glutathione reductase (GR) along with elevated S-metabolites (glutathione and methionine) to stabilize redox status under Fe-deficiency. Conclusions TH increases the availability and mobilization of Fe by inducing Fe-uptake pathways, which appears to help provide resistance to oxidative stress associated with Fe-shortage in soybean. Significance and Impact of the Study These findings indicate that while Fe deficiency does not affect the rate or degree of TH hyphal association in soybean roots, the beneficial effects of TH alone may be Fe deficiency-dependent.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

Transcriptomic data sets examining several stress responses in Zymomonas mobilis strains

We used RNA-seq to compare gene expression from Zymomonas mobilis ZM4 grown under various conditions: aerobic ± paraquat, anaerobic ± hydrogen peroxide, or an iron chelator. We analyzed two mutant strains lacking predicted transcription factors (ZMO_0442 and ZMO_1411) grown under aerobic or anaerobic conditions. We report the RNA-seq data from these experiments.

Bacterial Stress Response↗

DOE OSTI2020

Global Network Analysis of Neisseria gonorrhoeae Identifies Coordination between Pathways, Processes, and Regulators Expressed during Human Infection

Neisseria gonorrhoeae is a Gram-negative diplococcus that is responsible for the sexually transmitted infection gonorrhea, a high-morbidity disease in the United States and worldwide. Over the past several years, N. gonorrhoeae strains resistant to antibiotics used to treat this infection have begun to emerge across the globe. Thus, new treatment strategies are needed to combat this organism. Here, we utilized N. gonorrhoeae transcriptomic data sets, including those obtained from natural infection of the human genital tract, to infer the first global gene coexpression network of this pathogen. Interrogation of this network revealed genes central to the network that are likely critical for gonococcal growth, metabolism, and virulence, including genes encoding hypothetical proteins expressed during mucosal infection. In addition, network analysis revealed overlap in the response of N. gonorrhoeae to incubation with neutrophils and exposure to hydrogen peroxide stress in vitro. Network analysis also identified new targets of the gonococcal global regulatory protein Fur, while examination of the network neighborhood of genes allowed us to assign additional putative categories to several proteins. Collectively, the characterization of the first gene coexpression network for N. gonorrhoeae described here has revealed new regulatory pathways and new categories for proteins and has shown how processes important to gonococcal infection in both men and women are linked. This information fills a critical gap in our understanding of virulence strategies of this obligate human pathogen and will aid in the development of new treatment strategies for gonorrhea.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Editors’ Choice—Diffusion Media for Cation Contaminant Transport Suppression into Fuel Cell Electrodes

Polymer electrolyte membrane fuel cells provide an alternative option to fossil fuel-based energy conversion devices. However, the corrosion of fuel cell components, specifically the bipolar plates, introduces contaminants (e.g., Fe, Ni) into the membrane electrode assembly (MEA). These contaminants accelerate the ionomer degradation by acting as a Fenton’s reagent, decreasing the fuel cell’s durability. This study presents the mechanism and the diffusion media properties affecting the transport of cation contaminants into the MEA. Cation contaminant transport was studied after altering the gas diffusion layers (GDLs) wettability, emulating the GDL properties after prolonged operation, by ex situ hydrogen peroxide treatment or in situ electrochemical potential cycling. A GDL with crack-free microporous layer (MPL) showed a lower cation transport rate to the catalyst layer than MPL with cracks after both ex situ and in situ treatment. A novel GDL was developed from modification of the conventional GDL via the addition of a hydrophobic layer to the GDL substrate, which suppressed the contaminant cation transport significantly. This novel GDL also showed improved fuel cell performance.

25 ENERGY STORAGE↗

DOE OSTI2020

COVID-19 global pandemic planning: Performance and electret charge of N95 respirators after recommended decontamination methods

Shortages of N95 respirators for use by medical personnel have driven consideration of novel conservation strategies, including decontamination for reuse and extended use. Decontamination methods listed as promising by the Centers for Disease Control and Prevention (CDC) (vaporous hydrogen peroxide (VHP), wet heat, ultraviolet irradiation (UVI)) and several methods considered for low resource environments (bleach, isopropyl alcohol and detergent/soap) were studied for two commonly used surgical N95 respirators (3M™ 1860 and 1870+ Aura™). Although N95 filtration performance depends on the electrostatically charged electret filtration layer, the impact of decontamination on this layer is largely unexplored. As such, respirator performance following decontamination was assessed based on the fit, filtration efficiency, and pressure drop, along with the relationship between (1) surface charge of the electret layer, and (2) elastic properties of the straps. Decontamination with VHP, wet heat, UVI, and bleach did not degrade fit and filtration performance or electret charge. Isopropyl alcohol and soap significantly degraded fit, filtration performance, and electret charge. Pressure drop across the respirators was unchanged. Modest degradation of N95 strap elasticity was observed in mechanical fatigue testing, a model for repeated donnings and doffings. CDC recommended decontamination methods including VHP, wet heat, and UV light did not degrade N95 respirator fit or filtration performance in these tests. Extended use of N95 respirators may degrade strap elasticity, but a loss of face seal integrity should be apparent during user seal checks. NIOSH recommends performing user seal checks after every donning to detect loss of appropriate fit. Decontamination methods which degrade electret charge such as alcohols or detergents should not be used on N95 respirators. The loss of N95 performance due to electret degradation would not be apparent to a respirator user or evident during a negative pressure user seal check.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2025

Chelator-mediated Fenton post-treatment enhances methane yield from lignocellulosic residues via microbial community modulation

Advancing biomethane production from anaerobic digestion (AD) is essential for building a more reliable and resilient bioenergy system. However, incomplete conversion of lignocellulose-rich agricultural waste remains a key limitation, often leaving energy-dense residues in the digestate by-product. In this study, we introduce a novel application of chelator-mediated Fenton (CMF) post-treatment to recover untapped biomethane potential from these recalcitrant residues, representing a significant departure from conventional pre-treatment strategies. By systematically varying pH, iron-chelator concentration, and hydrogen peroxide dosage, we identified reaction conditions (pH 6–8, 5 mM Fe 2+ -dihydroxybenzene, 3–4 wt.% H 2 O 2 ) that enhanced lignocellulose deconstruction and increased dissolved organic carbon (DOC) availability for methanogenesis. CMF post-treatment led to up to a tenfold increase in biomethane potential compared to untreated controls. Microbial community analysis revealed enrichment of cellulolytic species, suggesting enhanced hydrolytic activity as a driver of improved conversion. Application of the CMF post-treatment method to isolated poplar lignin further demonstrated its versatility for diverse lignocellulosic substrates. These findings position CMF post-treatment as a promising strategy to enhance AD efficiency and valorize digestate.

Martinez, Daniella Victoria [Sandia National Labor↗

DOE OSTI2024

Moving toward automated µFTIR spectra matching for microplastic identification: addressing false identifications and improving accuracy

Abstract Infrared spectroscopy is a widely used tool for studying microplastics and identifying microparticles. Researchers rely on spectral libraries to differentiate between synthetic and natural materials. Unfortunately, spectral library matching is not perfect, and best practices require researchers to use time consuming, manual peak matching to assess spectral matches. Moving toward automated matching requires increased confidence in the matching process. Using spectra matching software may increase the efficiency of particle identification, however some matching strategies may confuse natural materials such as cotton, silk, and plant matter with common classes of synthetics such as polyesters and polyamides. In this experiment, we prepared 22 pristine sample materials from natural and synthetic sources and measured micro-Fourier transform infrared (µFTIR) spectra in transmission mode for each sample using a Thermo Nicolet iN10 MX instrument. The collected spectra were then input into two spectral library matching systems (Omnic Picta and Open Specy), using a total of five identification routines. Next, we placed a subset of four pristine microplastic materials in a biologically active river system for two weeks to simulate environmental samples. These simulated environmental samples were processed using 10% hydrogen peroxide for 24 h to remove organic contamination and then identified using the strongest performing library. We found that libraries with fewer sample spectra produced lower correlation matches and that using derivative correction greatly reduced the number of inaccuracies in identifying materials as either natural or synthetic. We also found that environmental fouling reduced the correlation value of library matches when compared to pristine particles, however the effect was not consistent across the four materials tested. Overall, we found that the accuracy of automated library matching in the tested systems and processing routines varied from 64.1 to 98.0% for distinguishing between natural and synthetic materials, and that a high Hit Quality Index (HQI) did not always correlate with accuracy. These results are important for the microplastic field, demonstrating a need to rigorously test spectral libraries and processing routines with known materials to ensure identification accuracy.

Kozloski, Rachel↗

DOE OSTI2021

Data from Reactive Species and Reaction Pathways for the Oxidative Cleavage of 4-Octene and Oleic Acid with H2O2 over Tungsten Oxide Catalysts

Oxidative cleavage of carbon–carbon double bonds (C═C) in alkenes and fatty acids produces aldehydes and acids valued as chemical intermediates. Solid tungsten oxide catalysts are low cost, nontoxic, and selective for the oxidative cleavage of C═C bonds with hydrogen peroxide (H2O2) and are, therefore, a promising option for continuous processes. Despite the relevance of these materials, the elementary steps involved and their sensitivity to the form of W sites present on surfaces have not been described. Here, we combine in situ spectroscopy and rate measurements to identify significant steps in the reaction and the reactive species present on the catalysts and examine differences between the kinetics of this reaction on isolated W atoms grafted to alumina and on those exposed on crystalline WO3 nanoparticles. Raman spectroscopy shows that W–peroxo complexes (W–(η2-O2)) formed from H2O2 react with alkenes in a kinetically relevant step to produce epoxides, which undergo hydrolysis at protic surface sites. Subsequently, the CH3CN solvent deprotonates diols to form alpha-hydroxy ketones that react to form aldehydes and water following nucleophilic attack of H2O2. Turnover rates for oxidative cleavage, determined by in situ site titrations, on WOx–Al2O3 are 75% greater than those on WO3 at standard conditions. These differences reflect the activation enthalpies (ΔH‡) for the oxidative cleavage of 4-octene that are much lower than those for the isolated WOx sites (36 ± 3 and 60 ± 6 kJ·mol–1 for WOx–Al2O3 and WO3, respectively) and correlate strongly with the difference between the enthalpies of adsorption for epoxyoctane (ΔHads,epox), which resembles the transition state for epoxidation. The WOx–Al2O3 catalysts mediate oxidative cleavage of oleic acid with H2O2 following a mechanism comparable to that for the oxidative cleavage of 4-octene. The WO3 materials, however, form only the epoxide and do not cleave the C–C bond or produce aldehydes and acids. These differences reflect the distinct site requirements for these reaction pathways and indicate that acid sites required for diol formation are strongly inhibited by oleic acids and epoxides on WO3 whereas the Al2O3 support provides sites competent for this reaction and increase the yield of the oxidative cleavage products.

Catalysis↗

DOE OSTI2022

Data for Catalyst and Reactor Design Considerations for Selective Production of Acids by Oxidative Cleavage of Alkenes with H2O2

Oxidative cleavage of alkenes and unsaturated fatty acids with hydrogen peroxide gives an efficient and sustainable process to obtain mono- and di-acids for polymers and lubricants with fewer safety risks and less environmental impact than processes that utilize ozone or other inorganic oxidizers (e.g., permanganate, dichromate, etc.). Guided by insight into the mechanisms for competing reaction pathways (i.e., epoxidation of alkene on W–(η2-O2) complexes vs. H2O2 decomposition) and the apparent kinetics derived from kinetic experiments, here, we postulate that W-based heterogeneous catalysts can provide high performance and stable operations at low H2O2 concentrations. Semi-batch reactors with continuous introduction of H2O2 solutions offer the means to maintain low H2O2 concentrations while providing sufficient quantities of H2O2 to satisfy the reaction stoichiometry. We derived simple kinetic model equations for the epoxidation, ring-opening, oxidative cleavage, and oxidation steps and fit theses equations to batch experimental data to obtain kinetic parameters. This kinetic model describes the concentration profiles of reactant, oxidant, and products well as shown by agreement with experimental data. Further predictions of the optimal H2O2 feed rate for semi-batch operation utilized by the proposed rate expressions and the reactor design equations suggest that low H2O2 feed rate increases selectivity towards oxidative cleavage products and selective use of H2O2 for oxidative cleavage pathway. Comparisons of oxidative cleavage of 4-octene in batch and semi-batch reactors show that semi-batch reactors with optimized molar feed rates of H2O2 increased oxidative cleavage product selectivities (76% to 99%; with an increase in butyric acid selectivity from 1% to 55%) and H2O2 selectivity (3% to 30%). In addition, semi-batch reaction conditions used avoid H2O2-mediated dissolution of W-atoms from the catalyst. Analysis of these findings suggest that solid oxide catalysts will be effective for continuous oxidative cleavage reactions if deployed within fixed-bed reactors that allow for distributed introduction of reactants and therefore low in situ concentrations of H2O2.

Catalysis↗

DOE OSTI2022

Effects of physical, chemical, and biological ageing on the mineralization of pine wood biochar by a Streptomyces isolate

If biochar is to be used for carbon (C) management, we must understand how weathering or ageing affects biochar C mineralization. Here, we incubated aged and unaged eastern white pine wood biochar produced at 350 and 550°C with a Streptomyces isolate, a putative biochar-decomposing microbe. Ageing was accelerated via three different processes, namely, (a) physical ageing–subjecting biochar to alternating freeze-thaw and wet-dry cycles, (b) chemical ageing–treating biochar with concentrated hydrogen peroxide and (c) biological ageing–incubating biochar in the presence of nutrients and microorganisms. Elemental composition and surface chemistry (Fourier Transform Infrared spectroscopy) of biochar samples were compared before and after ageing. Biochar C mineralization between ageing treatments was significantly different in the case of 350°C biochar ( p value = 0.03). Among the 350°C biochars, physical ageing resulted in the greatest increase (by 103%) in biochar C mineralization ( p value = 0.05). However, in the case of 550°C biochar, ageing did not result in a significant change in biochar C mineralization ( p value = 0.40). Biochar C mineralization was positively correlated with an increase in O/C ratio post-ageing ( r s = 0.86, p value = 0.01). In the case of 350°C biochar, surface oxidation during ageing enhanced biochar degradation by the isolate. For 550°C biochar, however, ageing did not significantly increase biochar C mineralization, likely due to high condensed aromatic C content and lower surface oxidation during ageing. The results from our study suggest that low temperature aged biochar is more susceptible to biological degradation by soil microbes. These findings have implications for the use of biochar for long term C storage in soils.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Materials Data on O2 by Materials Project

O2 is alpha oxygen-like structured and crystallizes in the monoclinic C2/m space group. The structure is zero-dimensional and consists of eight hydrogen peroxide molecules. O is bonded in a single-bond geometry to one O atom. The O–O bond length is 1.23 Å.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Materials Data on H11O8 by Materials Project

(H2O)2(H2O2)3(H3O2)4 crystallizes in the triclinic P1 space group. The structure is zero-dimensional and consists of one hydrogen peroxide hydrate molecule, one water molecule, and two water water molecules.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Materials Data on Si6O13 by Materials Project

(SiO2)12O2 is Low Tridymite-like structured and crystallizes in the hexagonal P6/mcc space group. The structure is three-dimensional and consists of two hydrogen peroxide molecules and one SiO2 framework. In the SiO2 framework, Si is bonded to four O atoms to form corner-sharing SiO4 tetrahedra. There is three shorter (1.62 Å) and one longer (1.63 Å) Si–O bond length. There are four inequivalent O sites. In the first O site, O is bonded in a bent 150 degrees geometry to two equivalent Si atoms. In the second O site, O is bonded in a bent 150 degrees geometry to two equivalent Si atoms. In the third O site, O is bonded in a linear geometry to two equivalent Si atoms. In the fourth O site, O is bonded in a bent 150 degrees geometry to two equivalent Si atoms.

36 MATERIALS SCIENCE↗