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All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Chemistry of Cu(acac){sub 2} on Ni(110) and Cu(110) surfaces: Implications for atomic layer deposition processes

The thermal chemistry of copper(II)acetylacetonate, Cu(acac){sub 2}, on Ni(110) and Cu(110) single-crystal surfaces was probed under vacuum by using x-ray photoelectron spectroscopy (XPS) and temperature programmed desorption (TPD). Some data for acetylacetone (Hacac, CH{sub 3}COCH{sub 2}COCH{sub 3}) adsorbed on Ni(110) are also reported as reference. Chemical transformations were identified in several steps covering a temperature range from 150 K to at least 630 K. The desorption of Hacac and a 3-oxobutanal (CH{sub 3}COCH{sub 2}CHO) byproduct was observed first at 150 and 180 K on Ni(110) and at 160 and 185 K on Cu(110), respectively. Partial loss of the acetylacetonate (acac) ligands and a likely change in adsorption geometry are seen next, with the possible production of HCu(acac), which desorbs at 200 and 235 K from the nickel and copper surfaces, respectively. Molecular Cu(acac){sub 2} desorption is observed on both surfaces at approximately 300 K, probably from recombination of Cu(acac) and acac surface species. The remaining copper atoms on the surface lose their remaining acac ligands to the substrate and become reduced directly to metallic copper. At the same time, the organic ligands follow a series of subsequent surface reactions, probably involving several C-C bond-scissions, to produce other fragments, additional Hacac and HCu(acac) in the gas phase in the case of the copper surface, and acetone on nickel. A significant amount of acac must nevertheless survive on the surface to high temperatures, because Hacac peaks are seen in the TPD at about 515 and 590 K and the C 1s XPS split associated with acac is seen up to close to 500 K. In terms of atomic layer deposition processes, this suggests that cycles could be design to run at such temperatures as long as an effective hydrogenation agent is used as the second reactant to remove the surface acac as Hacac. Only a small fraction of carbon is left behind on Ni after heating to 800 K, whereas more carbon and additional oxygen remains on the surface in the case of Cu.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Thermal chemistry of the Cu-KI5 atomic layer deposition precursor on a copper surface

The thermal chemistry of a Cu(I) ketoiminate complex, Cu-KI5, resulting from the modification of the known Air Products CupraSelect{sup ®} copper CVD precursor Cu(hfac)(tmvs) designed to tether the two ligands via an isopropoxide linker, was studied under ultrahigh vacuum on a Cu(110) single-crystal surface by using a combination of temperature programmed desorption (TPD) and x-ray photoelectron spectroscopy. Adsorption at low temperatures was determined to take place via the displacement of the vinyl ligand by the surface. Molecular desorption was seen at 210 K, and the evolution of Cu(II)-KI5{sub 2} was established to take place at 280 K, presumably from a disproportionation reaction that also leads to the deposition of Cu(0). Other sets of desorption products were seen at 150, 250, and 430 K, all containing copper atoms and small organic moieties with molecular masses below 100 amu. The latter TPD peak in particular indicates significant fragmentation of the ligands, likely at the C–N bond that holds the vinylsilane-isopropoxide moiety tethered to the ketoimine fragment, and possibly also at the union between the vinylsilane and the alkoxide linker. The 430 K temperature measured for this chemistry may set an upper limit for clean Cu film deposition, but since reactivity on the surface was also found to be inhibited at higher surface coverages, it may be delayed to higher temperatures under atomic layer deposition conditions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Surface structure and surface kinetics of InN grown by plasma-assisted atomic layer epitaxy: A HREELS study

The surface bonding configuration and kinetics of hydrogen desorption from InN grown by plasma-assisted atomic layer epitaxy have been investigated. High resolution electron energy loss spectra exhibited loss peaks assigned to a Fuchs–Kliewer surface phonon, N-N and N-H surface species. The surface N-N vibrations are attributed to surface defects. The observation of N-H but no In-H surface species suggested N-terminated InN. Isothermal desorption data were best fit by the first-order desorption kinetics with an activation energy of (0.88 ± 0.06) eV and pre-exponential factor of (1.5 ± 0.5) × 10{sup 5 }s{sup −1}.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Preheating temperature effect on tritium retention in VPS-W

The W coating by Vacuum Plasma Spraying (VPS) technology is thought to be reasonable for most plasma facing components in future fusion reactors. In this paper the deuterium retention behavior for the Vacuum Plasma Spraying (VPS) tungsten (W) coating has been studied to demonstrate the tritium retention as a function of heating temperature. It has been found that two major deuterium desorption stages were observed at the temperature regions of 400 - 700 K (Stage 1) and 900 - 1100 K (Stage 2), considering that Stage 1 has been linked to the desorption of deuterium trapped by near surface and intrinsic defects, and Stage 2 has been related to the desorption of deuterium bound to impurities as C-D bonds. By heating the sample above 673 K, the major peak of C-1s shifted from C-O bond to C-C bond, where the retention of deuterium as Stage 2 has increased. Therefore it indicates that the hydrogen isotope retention was controlled by the amount of C-C bond in VPS, most of which was contaminated during the VPS coating process. The comparison of several samples (VPS-W with shading, VPS-W without shading and Polycrystalline W (PCW)) shows that the carbon impurity has a large affinity with deuterium and makes stable trapping states compared to that with intrinsic defects and grain boundaries. However, most of them was reduced by heating at 1173 K. Therefore, heating treatment is quite important to get rid of carbon impurities and refrain higher tritium retention in VPS. (authors)

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2011

STRONTIUM AND ACTINIDE SORPTION BY MST AND MMST UNDER CONDITIONS REVELANT TO THE SMALL COLUMN ION-EXCHANGE PROCESS

A series of tests were performed to examine the kinetics of Sr and actinide removal by monosodium titanate (MST) and modified monosodium titanate (mMST) under mixing conditions similar to what will be provided in the Small Column Ion Exchange (SCIX) Program. Similar removal kinetics were seen for two different mixing energies, indicating that under these conditions bulk solution transport is not the rate limiting step for Sr and actinide removal. Sr removal was found to be rapid for both MST and mMST, reaching steady-state conditions within six hours. In contrast, at least six weeks is necessary to reach steady-state conditions for Pu with MST. For mMST, steady-state conditions for Pu were achieved within two weeks. The actual contact time required for the SCIX process will depend on starting sorbate concentrations as well as the requirements for the decontaminated salt solution. During testing leaks occurred in both the MST and mMST tests and evidence of potential desorption was observed. The desorption likely occurred as a result of the change in solids to liquid phase ratio that occurred due to the loss of solution. Based on these results, Savannah River National Laboratory (SRNL) recommended additional testing to further study the effect of changing phase ratios on desorption. This testing is currently in progress and results will be documented in a separate report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Xe Concentration Activity

INL conducted extensive studies to understand how the Xe capacity of AgZ-PAN changes under various conditions including flowrate, temperature, concentration, carrier gas, and irradiation of the sorbent. Therefore, it is well understood that AgZ-PAN can capture Xe under a wide range of conditions. While these studies were performed to prove that Xe can be completely desorbed from the column, the ability to concentrate Xe during desorption was not studied. Concentrating Xe during desorption would be ideal so as to produce Xe that can be used for commercial and research applications. This report investigates the Xe concentrating potential of AgZ-PAN by running multiple Xe adsorption-desorption cycles, collecting the desorbed effluent from a saturated AgZ-PAN column, and then loading it onto a fresh column.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2018

Understanding Mercury's Exosphere: Models Derived from MESSENGER Observations: Chapter - 15

The observations of Mercury's exosphere described in Chapter 14 have led to many modeling efforts. Early models were based upon a few simple assumptions and primarily explored the dynamics of sodium atoms pushed anti-sunward by radiation pressure [Ip, 1986; Smyth and Marconi, 1995]. More recently, these early models have been superseded by simulations with an increasing number of interdependent source processes [Leblanc and Johnson, 2003; Mura et al., 2009; Leblanc and Johnson, 2010; Burger et al., 2010, 2012, 2014]. We briefly summarize the source and loss processes before describing the published exosphere models, first for the three species observed almost continuously during the MESSENGER mission by the Ultraviolet and Visible Spectrometer (UVVS) channel of the Mercury Atmospheric and Surface Composition2Spectrometer (MASCS), (Na, Mg and Ca), and then more briefly for other species that have been observed or for which new upper limits have been derived.15.1 Overview of Source and Loss Processes15.1.1 Source Processes15.1.1.1 Thermal DesorptionThermal desorption (or thermal evaporation) is the release of adsorbed atoms from a surface via heating. Thermal desorption is related to the binding energy of the atom on the surface and the vibrational frequency of the bound atom, such that the rate of thermal desorption is given by, (15.1)where TD,

Thermal↗
DOE OSTI2011

Adsorption and Reaction of C1-C3 Alcohols over CeOx(111) Thin Films

This study reports the interaction of methanol, ethanol, 1-propanol, and 2-propanol with well-ordered CeO{sub 2}(111) thin film surfaces. All of the alcohols adsorb at low temperature by forming alkoxy and hydroxyl species on the surface. On fully oxidized CeO{sub 2}(111), recombination occurs between some of the alkoxys and hydroxyls, resulting in alcohol desorption near 220 K. At the same temperature, some of the surface hydroxyls disproportionate to produce water and the loss of lattice O. The remaining alkoxys react above 550 K. The primary alcohols favor dehydrogenation products (aldehydes). There is a net loss of O from the system, resulting in a reduction of the ceria. The secondary alcohol, 2-propanol, undergoes primarily dehydration, producing propene with no net change in the cerium oxidation state. Reduced CeO{sub x}(111) competes with the gaseous products for available O. Little or no water is produced. The reaction selectivity for the C{sub 2} and C{sub 3} alcohols shifts toward favoring dehydration products. The loss of O from the alcohols leads to oxidation of the reduced ceria. Compared with the oxidized surface, the alkene desorption shifts to lower temperature, whereas the aldehyde desorption shifts to higher temperature. This indicates that, on the reduced surface, it is easier to break the C-O bond but more difficult to break the O-substrate bond.

10 SYNTHETIC FUELS↗
DOE OSTI2012

Remediation of Mercury Contaminated Soils at the Miramas Site - 12243

Beneficial 'new' use of the Miramas Site is the remediation objective for a former light isotope manufacturing facility. Remediation operations will remove contaminated soils and materials and deconstruct facilities. The remediation objective is faced with project challenges and regulatory requirements that dictate/influence the outcome. The operation consists of the remediation of approximately 100,000 cubic meters of soil and the decommissioning of facilities. The types and ranges of waste are the result of historical processing activities (chemical facilities, pyrotechnic components storage, mining component treatment and light isotope manufacturing activities). Mercury is the primary component of the waste, but metals and organic compounds are also possible waste components. A thermal desorption process is used to remove Mercury from the polluted soil while a biological treatment is considered to the organic nitrate compound removal. A focus is done on the technologies used to remediate the Mercury contaminated soil. After few months of operation, the first results confirm that the technology choices were relevant and the soil remediation project is a success. The first successful month of operation at an industrial scale demonstrate that the Thermal Desorption is an efficient and relevant process to remediate large quantity of mercury contaminated soils. The project is on cost and the mercury removal should be end by 2014. The scrubbing is a good way to limit the volume of material to be treated with the Thermal Desorption Unit. The biological treatment is a promising process for the organic nitrate compound removal and testing at a pilot scale will be done in 2012. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Consequences of Intrapore Liquids on Reactivity, Selectivity, and Stability for Aldol Condensation Reactions on Anatase TiO 2 Catalysts

Abstract This study provides evidence and mechanistic interpretations for the significant consequences of intrapore non‐polar liquids on acetone aldol condensation turnover rates, selectivity to primary dimer products, and catalyst stability for reactions at Lewis acid‐base site pairs on TiO 2 surfaces. These non‐polar liquids confer such benefits through the preferential stabilization of transition states (TS) for adsorption (“entry”) and desorption (“exit”) steps, which place their respective reactants or products within a solvating outer sphere environment. The extent to which non‐polar fluids ( n ‐heptane) form an intrapore liquid phase within TiO 2 voids was obtained from N 2 uptakes using established formalisms that consider the different molal volume, surface tension, and volatility between N 2 and n ‐heptane. Acetone condensation rates are limited by C−H activation, an “entry” step that forms bound prop‐1‐en‐2‐olates via a TS stabilized by intrapore liquids, leading to higher aldol condensation turnover rates as n ‐heptane pressure increases and active TiO 2 surfaces become increasingly immersed within a non‐polar liquid phase. These liquids solvate the late TS structures that mediate the desorption of primary C 6 condensation products even more effectively than those involved in prop‐1‐en‐2‐olate formation or in nucleophilic attack events that later form C−C bonds. Such preferential solvation favors desorption over C−C coupling events, thus disfavoring the formation of larger oligomers that become stranded at active sites, thus leading to much slower deactivation. Moreover, solvation by non‐polar liquids also leads to C 6 alkanones as the sole products formed in a single surface sojourn. These effects of a non‐polar dense phase circumvent the inherent stability, reactivity, and selectivity hurdles that have precluded practical aldol condensation catalysis on Lewis acid‐base pairs at oxide surfaces; these consequences are demonstrated here for TiO 2 catalysts, acetone aldol condensation reactions, and n ‐heptane as the non‐polar liquid but through strategies, concepts, and mechanistic features that extend to other systems. More generally, these observations and their mechanistic origins demonstrate how a contacting liquid preferentially solvates TS structures for elementary steps that involve either reactants arriving from or products entering into an outer sphere environment that contains a dense non‐polar phase.

Kadam, Shashikant A.↗
DOE OSTI2015

Bioaccessibility of Cd and Pb in tailings from a zinc smelting in Brazil: implications for human health

Soils and wastes enriched with heavy metals may present significant ecological and human health risks. A considerable number of mining/smelting areas exist in Brazil, where high levels of metals have been found, as well as in their surrounding soils and sediments. However, studies of bioaccessibility of metals in soils/tailings from these areas are scarce, despite their potential informational contribution concerning exposure risks for residents near these areas. This study evaluated tailing samples collected from four sites of a smelting area aiming to: (i) evaluate the presence of metals of potential concern; (ii) investigate Cd and Pb bioaccessibility; and, (iii) determine the desorption kinetics of Cd and Pb. Five composite samples were collected from each site, at two depths, from a zinc smelting area located near Três Marias city - MG, Brazil. Availability of Cd and Pb was measured using a bioaccessibility test and a desorption experiment. High concentrations of total Cd and Pb and great variability were found in the tailings (up to 1743 mg Cd kg -1 and 8675 mg Pb kg -1 ), indicating the importance of adequate planning for their final disposal, in order to avoid contamination in the surrounding environment. Cadmium and Pb bioaccessibility percentages in the intestinal phase were less than 47 and 4%, respectively, which represents significant fractions not available for absorption in the intestinal tract. However, this material has to be monitored since its bioaccessibility may increase with eventual physicochemical changes, releasing Cd and Pb. Desorption kinetics experiments revealed that the Pb in the samples remained in less labile fractions whereas Cd was found in more labile fractions, which is in accordance with the bioaccessibility result.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Alkaline zirconates as effective materials for hydrogen production through consecutive carbon dioxide capture and conversion in methane dry reforming

In this work, H 2 production was evaluated using different carbonation conditions and two alkaline zirconates. For this purpose, Li 2 ZrO 3 and Na 2 ZrO 3 were synthesized, characterized and tested on a consecutive process composed of initial CO 2 capture, followed by methane dry reforming (MDR). Thermogravimetric results showed that under the four gas mixtures tested (diluted and saturated CO 2 , CO and CO-O 2 ), both ceramics are able to chemisorb CO 2 , with Na2ZrO3 having the highest capture with saturated CO 2 . In catalytic tests, ceramics carbonated with saturated CO 2 or CO-O 2 gas flows were able to act as sorbents and catalysts, producing H 2 at T > 750 °C through the partial oxidation of methane. This reaction was produced because CO2 desorption did not occur, thus avoiding the MDR process. On the other hand, carbonated ceramics under a CO-O2 gas mixture presented an outstanding catalytic performance. Between 450 and 750 °C, H 2 was formed through the MDR process promoted by CO 2 desorption from both ceramics. This result is in line with CO 2 desorption results, where a weaker CO 2 –solid interaction was observed in comparison with saturated CO 2 2. Afterward, both ceramics presented a similar catalytic behavior, good regeneration and cyclability after the double process proposed (CO 2 capture-MDR reaction). Lithium zirconate also presented high thermal stability during cycle tests; meanwhile, sodium zirconate showed an important H 2 production increase as a function of cycles. Finally, both materials are feasible options for producing a clean energy source in a moderate temperature range through the catalytic conversion of two greenhouse gases (CO 2 and CH 4 ).

03 NATURAL GAS↗
DOE OSTI2014

Direct molecular diffusion and micro-mixing for rapid dewatering of LiBr solution

A slow molecular diffusion rate often limits the desorption process of an absorbate molecule from a liquid absorbent. To enhance the desorption rate, the absorbent is often boiled to increase the liquid vapor interfacial area. However, the growth of bubbles generated during the nucleate boiling process still remains mass-diffusion limited. Here, it is shown that a desorption rate higher than that of boiling can be achieved, if the vapor absorbent interface is continuously replenished with the absorbate-rich solution to limit the concentration boundary layer growth. The study is conducted in a LiBr-water-solution, in which the water molecules' diffusion rate is quite slow. The manipulation of the vapor solution interface concentration distribution is enabled by the mechanical confinement of the solution flow within microchannels, using a hydrophobic vapor-venting membrane and the implementation of microstructures on the flow channel's bottom wall. The microstructures stretch and fold the laminar streamlines within the solution film and produce vortices. The vortices continuously replace the concentrated solution at the vapor solution interface with the water-rich solution brought from the bottom and middle of the flow channel. The physics of the process is described using a combination of experimental and numerical studies. Published by Elsevier Ltd.

Bigham, S↗
DOE OSTI2022

Sorbent-based oxygen separation with YBC114 for energy storage systems

In our report we aimed to design, build, and evaluate an oxygen separation system to provide an inert sweep gas with low oxygen partial pressure (pO2) to redox-active thermochemical energy conversion reactors for a range of applications, including two-step redox cycles for thermochemical energy storage, water splitting, and carbon-dioxide splitting. The separation is based on an oxygen-selective sorbent, YBaCo4O7+δ (YBC114), which has excellent oxygen sorption and desorption properties demonstrated in our previous work. The oxygen separation performance of YBC114 was comprehensively studied by thermogravimetric analysis, sorption breakthrough experiments, and temperature swing sorption - desorption cycles. The results reveal that YBC114 can produce inert sweep gas with an oxygen concentration of less than 100 ppmv for at least 20 min during the thermal swing adsorption (TSA) cycle with the current sorption bed configuration, and the performance is consistent from cycle to cycle. The optimal sorption and desorption temperatures for the TSA process with YBC114 are determined to be 300 °C and 500 °C, respectively. Although challenges remain for the current separation system (e.g., high sorption temperature and slow kinetics), this study demonstrates the potential to use the oxygen-selective sorbent to produce an inert sweep gas, the feasibility of the oxygen separation concept, and guides new sorbent material development to make this application economically practical. A simple procedure is described for designing the YBC114 oxygen separation process.

42 ENGINEERING↗
DOE OSTI2016

Oral relative bioavailability of Dichlorodiphenyltrichloroethane (DDT) in contaminated soil and its prediction using in vitro strategies for exposure refinement

In this study, the bioavailability of DDTr (sum of DDT, DDD and DDE isomers) in pesticide-contaminated soil was assessed using an in vivo mouse model. DDTr relative bioavailability (RBA) ranged from 18.7±0.9 (As35) to 60.8±7.8% (As36) indicating that a significant portion of soil-bound DDTr was not available for absorption following ingestion. When DDTr bioaccessibility was assessed using the organic Physiologically Based Extraction Test (org-PBET), the inclusion of a sorption sink (silicone cord) enhanced DDTr desorption by up to 20-fold (1.6–3.8% versus 18.9–56.3%) compared to DDTr partitioning into gastrointestinal fluid alone. Enhanced desorption occurred as a result of the silicone cord acting as a reservoir for solubilized DDTr to partition into, thereby creating a flux for further desorption until equilibrium was achieved. When the relationship between in vivo and in vitro data was assessed, a strong correlation was observed between the mouse bioassay and the org-PBET+silicone cord (slope=0.94, y-intercept=3.5, r{sup 2}=0.72) suggesting that the in vitro approach may provide a robust surrogate measure for the prediction of DDTr RBA in contaminated soil. - Highlights: • An optimised mouse assay was used to quantify DDTr relative bioavailability in soil. • DDTr bioaccessibility was also determined using an in vitro sorption sink approach. • A strong correlation was observed between in vivo and in vitro data. • The sorption sink approach may be used to predict DDTr relative bioavailability.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2013

Nanofibrous membrane-based absorption refrigeration system

This paper presents a study on the efficacy of highly porous nanofibrous membranes for application in membrane-based absorbers and desorbers. Permeability studies showed that membranes with a pore size greater than about one micron have a sufficient permeability for application in the absorber heat exchanger. Membranes with smaller pores were found to be adequate for the desorber heat exchanger. The membranes were implemented in experimental membrane-based absorber and desorber modules and successfully tested. Parametric studies were conducted on both absorber and desorber processes. Studies on the absorption process were focused on the effects of water vapor pressure, cooling water temperature, and the solution velocity on the absorption rate. Desorption studies were conducted on the effects of wall temperature, vapor and solution pressures, and the solution velocity on the desorption rate. Significantly higher absorption and desorption rates than in the falling film absorbers and desorbers were achieved. Published by Elsevier Ltd.

Isfahani, RN↗
DOE OSTI2026

The presence of Ru metal modifies the behavior of deuterium bound to pyridinic nitrogen in doped graphene-like materials

We used a combination of x-ray photoelectron spectroscopy (XPS) and density functional theory (DFT) to investigate how the presence of a ruthenium (Ru) metal substrate modifies the N-D bond strength of the pyridinic nitrogen species in nitrogen (N)-doped graphene (Gr) on Ru(0001) compared to metal-free highly-oriented pyrolytic graphite (HOPG) substrate. The N-dopants were introduced through low-energy N+/N2+ irradiation. N is embedded in the carbon materials in two predominant configurations: as graphitic N (GN: N substituted in the hexagonal C lattice) and pyridinic N (PN: substitutional N adjacent to a C vacancy). XPS data showed that upon atomic deuterium (D) exposure at 220 K, the PN peak shifted to a higher binding energy by +1.2 eV for HOPG and +1.0 eV for N-doped graphene on Ru(0001), while the GN peak remained unchanged, indicating that the D atoms bound solely to pyridinic N. 85% of PN sites on HOPG can be saturated with D atoms, whereas only ~30% of pyridinic N sites are able to bind D atoms in N-doped Gr/Ru(0001). Our DFT analysis shows that this difference is due to the coordination of PN to Ru atoms, which necessitates bond cleavage of the N-Ru interaction prior to D atom adsorption. D begins desorbing from N-HOPG at ~573 K and is fully desorbed by ~973 K, whereas desorption from N-doped graphene on Ru(0001) begins at ~290 K, with complete desorption observed at ~700 K, indicating that the Ru metal weakens the N-D bond strength. We also studied a high-surface-area, layered, and porous N-doped carbon material, internally labeled NC900, which was synthesized by pyrolysis of glucose and graphitic carbon nitride (g-C3N4) at 1173 K. D exposure caused a +1.1 eV PN peak shift in NC900, with no change in the GN peak. Moreover, the NC900 exhibited the same desorption behavior as HOPG, demonstrating that well-defined model systems can effectively capture the behavior of more complex N-doped carbon materials.

Alupothe Gedara, Buddhika S.↗