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DOE OSTI2018

Bragg coherent diffraction imaging of iron diffusion into gold nanocrystals

Understanding how diffusion takes place within nanocrystals is of great importance for their stability and for controlling their synthesis. In this study, we used the strain sensitivity of Bragg coherent diffraction imaging (BCDI) to study the diffusion of iron into individual gold nanocrystals in situ at elevated temperatures. The BCDI experiments were performed at the I-07 beamline at Diamond Light Source, UK. The diffraction pattern of individual gold nanocrystals was measured around the (11-1) Bragg peak of gold before and after iron deposition as a function of temperature and time. Phase retrieval algorithms were used to obtain real space reconstructions of the nanocrystals from their measured diffraction patterns. Alloying of iron with gold at sample temperatures of 300 °C–500 °C and dealloying of iron from gold at 600 °C were observed. The volume of the alloyed region in the nanocrystals was found to increase with the dose of iron. However, no significant time dependence was observed for the structure following each iron deposition, suggesting that the samples reached equilibrium relatively quickly. The resulting phase distribution within the gold nanocrystals after the iron depositions suggests a contraction due to diffusion of iron. Furthermore, our results show that BCDI is a useful technique for studying diffusion in three dimensions and alloying behaviour in individual crystalline grains.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Single gold atoms stabilized on nanoscale metal oxide supports are catalytic active centers for various reactions

Key recent findings that demonstrate that single‐gold atom sites stabilized on various oxide supports by –O bonds are the unique catalytic sites for a number of reactions, including the water‐gas shift reaction, methanol partial oxidation and steam reforming reactions, and the selective dehydrogenation of ethanol are summarized herein. Atomic dispersion of gold on various metal oxides was followed with aberration‐corrected high angle annular dark field/scanning transmission microscopy imaging and x‐ray absorption spectroscopy (XANES/EXAFS). Gold nanoparticles and subnanometer clusters are active only through their interfacial atoms directly interacting with the support, hence if present, they entail precious metal waste. From a design perspective, the important feature in these supported catalysts is the creation of many single‐site gold species anchored on the oxide support to maximize activity. Atomic gold‐centered catalyst designs afford 100% atom efficiency, and more importantly, have distinct product selectivity, different from that of extended metal surfaces. Novel experimental synthesis methods of atomically dispersed Au catalysts are discussed, which pave the way for the efficient use of precious metals, broadening the application of properly designed gold and other precious metals (Pt, Pd) to different reactions in energy conversion and green chemicals production. © 2015 American Institute of Chemical Engineers AIChE J , 62: 429–439, 2016

Wang, Chongyang↗

DOE OSTI2014

Transformation of thiolated chitosan-templated gold nanoparticles to huge microcubes

Graphical abstract: - Highlights: • Mercapto groups were grafted to chitosan molecule by a reactive amine reduction. • Functional polymer with well-defined monomer units controls AuNPs assembly. • Assembled morphologies depend on the ratio of AuNPs to thiolate groups. • Microcubes with side length of ∼20 μm was synthesized through a dialysis step. • A edge-to-middle growth mechanism of gold microcubes was observed. - Abstract: The L-cysteine molecules were successfully grafted to the 2-amino group of chitosan by a reactive amine reduction, and the as-synthesized thiolated chitosan (TC) molecules were used as the templates to direct the self-assembly of gold nanoparticles and induce the transformation of these assemblies to gold microcubes through a deep-going dialysis. We found that the ratio of gold nanoparticles to TC molecules could greatly affect the shape of the assembled clusters. Different stages of these clusters and microstructures during the dialysis process were characterized by scanning electron microscope (SEM), and the microcubes with average side length of about 20 μm were successfully synthesized. According to the morphology evolution of the assembly, it could be concluded that the microcubes were formed from external to internal. The SERS area mapping images of microcubes and some clusters were also collected to study the formation mechanism of gold microcubes. Our work demonstrates a simple and highly effective way to assemble gold nanoparticles into microcubes with unique properties.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Monitoring the Stimulated Uncapping Process of Gold-Capped Mesoporous Silica Nanoparticles

To establish a new method for tracking the interaction of nanoparticles with chemical cleaving agents, we exploited the optical effects caused by attaching 5-10 nm gold nanoparticles with molecular linkers to large mesoporous silica nanoparticles (MSN). At low levels of gold loading onto MSN, the optical spectra resemble colloidal suspensions of gold. As the gold is removed, by cleaving agents, the MSN revert to the optical spectra typical of bare silica. Time-lapse images of gold-capped MSN stationed in microchannels reveal that the rate of gold release is dependent on the concentration of the cleaving agent. Finally, the uncapping process was also monitored successfully for MSN endocytosed by A549 cancer cells, which produce the cleaving agent glutathione. These experiments demonstrate that the optical properties of MSN can be used to directly monitor cleaving kinetics, even in complex cellular settings.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Population and hierarchy of active species in gold iron oxide catalysts for carbon monoxide oxidation

The identity of active species in supported gold catalysts for low temperature carbon monoxide oxidation remains an unsettled debate. With large amounts of experimental evidence supporting theories of either gold nanoparticles or sub-nm gold species being active, it was recently proposed that a size-dependent activity hierarchy should exist. Here we study the diverging catalytic behaviors after heat treatment of Au/FeO x materials prepared via co-precipitation and deposition precipitation methods. After ruling out any support effects, the gold particle size distributions in different catalysts are quantitatively studied using aberration corrected scanning transmission electron microscopy (STEM). A counting protocol is developed to reveal the true particle size distribution from HAADF-STEM images, which reliably includes all the gold species present. As a result, correlation of the populations of the various gold species present with catalysis results demonstrate that a size-dependent activity hierarchy must exist in the Au/FeO x catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Stabilization of 4H hexagonal phase in gold nanoribbons

Gold, silver, platinum and palladium typically crystallize with the face-centred cubic structure. Here we report the high-yield solution synthesis of gold nanoribbons in the 4H hexagonal polytype, a previously unreported metastable phase of gold. These gold nanoribbons undergo a phase transition from the original 4H hexagonal to face-centred cubic structure on ligand exchange under ambient conditions. Using monochromated electron energy-loss spectroscopy, the strong infrared plasmon absorption of single 4H gold nanoribbons is observed. Furthermore, the 4H hexagonal phases of silver, palladium and platinum can be readily stabilized through direct epitaxial growth of these metals on the 4H gold nanoribbon surface. Our findings may open up new strategies for the crystal phase-controlled synthesis of advanced noble metal nanomaterials.

Science & Technology - Other Topics↗

DOE OSTI2019

Single-atom gold oxo-clusters prepared in alkaline solutions catalyse the heterogeneous methanol self-coupling reactions

We report the direct use of inorganometallic gold complexes formed in alkaline solutions as robust heterogeneous catalysts. Specifically, mononuclear gold complexes with the gold atom surrounded by a shell of Na cations through -O- linkages were prepared by dissolving Au(OH) 3 in highly alkaline solutions of NaOH. The complexes remain intact upon impregnation onto supports or after drying in air to a crystalline powder. Supported catalysts containing exclusively atomic gold at loadings up to 1.2 wt.% Au were prepared. Either in supported or unsupported form, the mononuclear gold-centered oxo-clusters catalyze the selective methanol dehydrogenation reaction to methyl formate (MF) and hydrogen; a reaction of industrial interest as well as the key step in methanol steam reforming. The [Au1-Ox]- center was identified as the active catalytic site by experimental characterization and density functional theory studies. The methanol dehydrogenation reaction mechanism proceeds via the self-coupling of methanol to MF. No oxygen supply is necessary. Hence, hydrogen rather than water is produced at 2:1 (stoichiometric) molar ratio to MF. The dried crystalline powder of the solution was used as an unsupported catalyst, showing the same chemistry as the supported clusters. Ab initio molecular dynamics (AIMD) simulations of methanol self-coupling on the mononuclear gold clusters revealed the formation of formate spectators on the clusters under reaction conditions, also corroborated by in situ DRIFTS. The inclusion of these spectators proved crucial towards the accurate description of the energetics of self-coupling of methanol on these clusters, thus unravelling the nature of the active site. Catalyst stability up to 250-300 oC in reaction conditions is demonstrated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Cationic Gold Clusters Ligated with Differently Substituted Phosphines: Effect of Substitution on Ligand Reactivity and Binding

We present a systematic study of the effect of the number of methyl (Me) and cyclohexyl (Cy) functional groups in monodentate phosphine ligands on the solution-phase synthesis of ligated sub-nanometer gold clusters and their gas-phase fragmentation pathways. Small mixed ligand cationic gold clusters were synthesized using ligand exchange reactions between pre-formed triphenylphosphine ligated (PPh3) gold clusters and monodentate Me- and Cy-substituted ligands in solution and characterized using electrospray ionization mass spectrometry (ESI-MS) and collision-induced dissociation (CID) experiments. Under the same experimental conditions, larger gold-PPh3 clusters undergo efficient exchange of unsubstituted PPh3 ligands for singly Me- and Cy-substituted PPh2Me and PPh2Cy ligands. The efficiency of ligand exchange decreases with an increasing number of Me or Cy groups in the substituted phosphine ligands. CID experiments performed for a series of ligand-exchanged gold clusters indicate that loss of a neutral Me-substituted ligand is preferred over loss of a neutral PPh¬3 ligand while the opposite trend is observed for Cy-substituted ligands. The branching ratio of the competing ligand loss channels is strongly correlated with the electron donating ability of the phosphorous lone pair as determined by the relative proton affinity of the ligand. The results indicate that the relative ligand binding energies increase in the order PMe3 < PPhMe2 < PPh2Me < PPh3< PPh2Cy < PPhCy2< PCy3. Furthermore, the difference in relative ligand binding energies increases with the number of substituted PPh3-mMem or PPh3-mCym ligands (L) exchanged onto each cluster. This study provides the first experimental determination of the relative binding energies of ligated gold clusters containing differently substituted monophosphine ligands, which are important to controlling their synthesis and reactivity in solution. The results also indicate that ligand substitution is an important parameter that must be considered in theoretical modeling of these complex systems

Environmental Molecular Sciences Laboratory↗

DOE OSTI2024

Finding a needle in a haystack: quantitative HERFD-XRF imaging and HERFD-XANES characterization of trace platinum in gold solidi from the Late Roman and Byzantine Empires

High-Energy Resolution Fluorescence Detection X-Ray Fluorescence (HERFD-XRF) imaging and HERFD X-ray Absorption Near Edge Structure (XANES) spectroscopy are used to quantify and characterize trace platinum (Pt) in gold solidi from the Late Roman and Byzantine Empires. Historically, the elemental analysis of coins has been pivotal in distinguishing authentic artifacts from forgeries, elucidating minting practices, and understanding economic shifts. Notably, a new gold source with high platinum content appeared in the fourth century CE, transforming the Roman economy. Traditional methods struggled to detect platinum due to the overwhelming gold matrix. Here, this study demonstrates the effectiveness of HERFD techniques in resolving this challenge. Three gold solidi, minted between 654 and 659 CE, were analyzed alongside reference gold materials with known Pt concentrations. The HERFD-XRF imaging revealed spatial distributions of platinum, highlighting non-uniformities within the coins. Additionally, HERFD-XANES spectroscopy identified the oxidation states and chemical speciation of platinum. Results demonstrate that platinum in the solidi primarily exists as metallic Pt, with some surface oxidation. The findings align with previous measurements but reveal higher Pt concentrations and significant inhomogeneities. This research confirms the reliability of HERFD methods for quantifying trace elements and provides new insights into the raw material sources and minting techniques of ancient gold coins. The non-destructive nature of this approach allows for extensive analyses, offering valuable data for historical, economic, and archaeological studies. This innovative application of HERFD-XRF imaging and XANES in cultural heritage research underscores the potential for detailed material characterization and conservation, enhancing our understanding of ancient economies and trade patterns.

Van Loon, Lisa L.↗

DOE OSTI2025

Gold L-shell emission spectroscopy as a temperature diagnostic in laser-driven experiments

Measurements of plasma conditions within gold hohlraums are challenging but provide important information about hohlraum energy transport. To date, there are no reliable passive diagnostic approaches that produce information about the hohlraum plasma conditions. Gold L-shell emission spectroscopy is a promising method to measure the electron temperature in multi-keV gold hohlraum plasmas. In this study, we compare time-resolved measurements of gold L-shell spectra against a more conventional electron temperature-sensitive diagnostic, K-shell emission from zinc, a mid-Z dopant. The Au L-shell and Zn K-shell spectra are taken simultaneously. The analysis of both sets of data exhibits good agreement with a singular rad-hydro model, suggesting a similar evolution in the mean electron temperature of the hohlraum plasma. These findings support the use of L-shell spectroscopy of gold as a method to study gold plasma conditions.

Emission spectroscopy↗

DOE OSTI2014

Influence of photon beam energy on the dose enhancement factor caused by gold and silver nanoparticles: An experimental approach

Purpose: Noble metal nanoparticles have found several medical applications in the areas of radiation detection; x-ray contrast agents and cancer radiation therapy. Based on computational methods, many papers have reported the nanoparticle effect on the dose deposition in the surrounding medium. Here the authors report experimental results on how silver and gold nanoparticles affect the dose deposition in alanine dosimeters containing several concentrations of silver and gold nanoparticles, for five different beam energies, using electron spin resonance spectroscopy (ESR). Methods: The authors produced alanine dosimeters containing several mass percentage of silver and gold nanoparticles. Nanoparticle sizes were measured by dynamic light scattering and by transmission electron microscopy. The authors determined the dose enhancement factor (DEF) theoretically, using a widely accepted method, and experimentally, using ESR spectroscopy. Results: The DEF is governed by nanoparticle concentration, size, and position in the alanine matrix. Samples containing gold nanoparticles afford a DEF higher than 1.0, because gold nanoparticle size is homogeneous for all gold concentrations utilized. For samples containing silver particles, the silver mass percentage governs the nanoparticles size, which, in turns, modifies nanoparticle position in the alanine dosimeters. In this sense, DEF decreases for dosimeters containing large and segregated particles. The influence of nanoparticle size-position is more noticeable for dosimeters irradiated with higher beam energies, and dosimeters containing large and segregated particles become less sensitive than pure alanine (DEF < 1). Conclusions: ESR dosimetry gives the DEF in a medium containing metal nanoparticles, although particle concentration, size, and position are closely related in the system. Because this is also the case as in many real systems of materials containing inorganic nanoparticles, ESR is a valuable tool for investigating DEF. Moreover, these results alert to the importance of controlling the size-position of nanoparticles to enhance DEF.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

NASA NTRS2018

Gaps in Thermal Design Guidelines in the Goddard Space Flight Center GOLD Rules

The GSFC (Goddard Space Flight Center) GOLD Rules (Goddard Open Learning Design; GSFC-STD-1000) provide a reasonably comprehensive list of guidelines for the design and testing of spacecraft and instruments based on the long heritage of successful GSFC missions. In general, all GSFC missions are required to comply with the GOLD Rules across a number of subsystems or to seek waivers to particular GOLD rules where compliance is not practical, either due to the risk posture of a mission or the cost and/or schedule associated with compliance. In thermal subsystems, GOLD Rules are applied to design margins throughout the project life cycle and include temperature margins, heater power margins, and two-phase transport margins. However, no explicit guidance is provided for two thermal design aspects: heater control authority (for stability requirements) and cryogenic design margins (which are often not reasonable to express in terms of temperatures). This can lead to ambiguity and inconsistency among projects when demonstrating GOLD Rules compliance. Two current GSFC projects, TIRS-2 (Thermal InfraRed Sensor 2) and WFIRST (Wide Field InfraRed Survey Telescope), are both missions with cryogenic aspects and active thermal control for stability. This paper seeks to outline the characterization of cryogenic margins during the design process for TIRS-2 and WFIRST as well as the project derived guidelines for heater control authority margin. This effort serves as potential first steps for updating the GOLD Rules to address these two areas in guiding thermal designs at GSFC.

Modeling↗

NASA NTRS2023

Thermospheric Temperature and ΣO/N 2 Variations as Observed by GOLD and Compared to MSIS and WACCM-X Simulations During 2019–2020 at Deep Solar Minimum

The ultraviolet-imaging spectrograph that comprises Global-scale Observations of the Limb and Disk (GOLD) mission in geostationary orbit at 47.5°W longitude has taken full disk images at high cadence throughout the deep solar minimum period of 2019–2020. Synoptic (i.e., concurrent and spatially unified and resolved) observations of thermospheric temperature and composition at ∼150 km altitude are made for the first time, allowing GOLD to disambiguate temporal and spatial variations. Here we analyze the daytime effective temperature and column integrated O and N2 density ratio (ΣO/N 2 ) data simultaneously observed by GOLD over 120°W–20°E longitude and 60°S–60°N latitude from 13 October 2019 to 12 October 2020. Daily zonal mean values are calculated for each latitude and compared with NRLMSIS 2.0 and simulations from the Whole Atmosphere Community Climate Model with thermosphere and ionosphere extension (WACCM-X). On average, the GOLD observations show higher temperatures than Mass Spectrometer Incoherent Scatter radar (MSIS) and WACCM-X by ∼20–60 K (5%–10%) and 80–120 K (12%–18%), respectively. The ΣO/N 2 ratios observed by GOLD are larger than the MSIS results by ∼0.4 (40%) but smaller than the WACCM-X simulations by ∼0.3 (30%). The observed and modeled results are correlated at most latitudes (r = 0.4–0.8), and GOLD, MSIS, and WACCM-X all display a similar seasonal variation and change with latitude. WACCM-X simulates a larger annual variation in ΣO/N 2 , suggesting that the thermospheric circulation is overestimated and atmospheric waves and turbulence transport are not properly represented in the model.

Guiping Liu↗

NASA NTRS2023

Thermospheric Temperature and ΣO/N2 Variations as Observed by GOLD and Compared to MSIS and WACCM-X Simulations During 2019–2020 at Deep Solar Minimum

The ultraviolet-imaging spectrograph that comprises Global-scale Observations of the Limb and Disk (GOLD) mission in geostationary orbit at 47.5°W longitude has taken full disk images at high cadence throughout the deep solar minimum period of 2019–2020. Synoptic (i.e., concurrent and spatially unified and resolved) observations of thermospheric temperature and composition at ∼150 km altitude are made for the first time, allowing GOLD to disambiguate temporal and spatial variations. Here we analyze the daytime effective temperature and column integrated O and N 2 density ratio (ΣO/N 2 ) data simultaneously observed by GOLD over 120°W–20°E longitude and 60°S–60°N latitude from 13 October 2019 to 12 October 2020. Daily zonal mean values are calculated for each latitude and compared with NRLMSIS 2.0 and simulations from the Whole Atmosphere Community Climate Model with thermosphere and ionosphere extension (WACCM-X). On average, the GOLD observations show higher temperatures than Mass Spectrometer Incoherent Scatter radar (MSIS) and WACCM-X by ∼20–60 K (5%–10%) and 80–120 K (12%–18%), respectively. The ΣO/N2 ratios observed by GOLD are larger than the MSIS results by ∼0.4 (40%) but smaller than the WACCM-X simulations by ∼0.3 (30%). The observed and modeled results are correlated at most latitudes (r = 0.4–0.8), and GOLD, MSIS, and WACCM-X all display a similar seasonal variation and change with latitude. WACCM-X simulates a larger annual variation in ΣO/N 2 , suggesting that the thermospheric circulation is overestimated and atmospheric waves and turbulence transport are not properly represented in the model.

Guiping Liu↗

DOE OSTI2018

Nobler than the Noblest: Noncubic Gold Microcrystallites

Conventional gold comprising the cubic lattice is universally known for its stability. However, well known to chemists and metallurgists, this nobility is challenged by reagents such as aqua regia, which dissolve gold to form a salt solution. Among metals, mercury blends with gold to form amalgam, otherwise transition metals such as copper tend to interact with gold surfaces in electrochemical media. Herein, we report a combined experimental and theoretical investigation of the stability of Au microcrystallites bearing unconventional crystal lattices that exhibit enhanced stability towards Hg and aqua regia and practically no interaction with Cu during electroless plating. Undoubtedly, the unconventional gold is nobler.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Tunable trimers: Using temperature and pressure to control luminescent emission in gold(I) pyrazolate-based trimers

A systematic investigation into the relationship between the solid-state luminescence and the intermolecular Au∙∙∙Au interactions in a series of pyrazolate-based gold(I) trimers; tris(μ 2 -pyrazolato-N,N')-tri-gold(I) (1), tris(μ 2 -3,4,5-trimethylpyrazolato-N,N')-tri-gold(I) (2), tris(μ 2 -3-methyl-5-phenylpyrazolato-N,N')-tri-gold(I) (3) and tris(μ 2 -3,5-diphenylpyrazolato-N,N')-tri-gold(I) (4) has been carried out using variable temperature and high pressure X-ray crystallography, solid-state emission spectroscopy, Raman spectroscopy and computational techniques. Single-crystal X-ray studies show that there is a significant reduction in the intertrimer Au∙∙∙Au distances both with decreasing temperature and increasing pressure. In the four complexes, the reduction in temperature from 293 to 100 K is accompanied by a reduction in the shortest intermolecular Au∙∙∙Au contacts of between 0.04 and 0.08 Å. The solid-state luminescent emission spectra of 1 and 2 display a red shift with decreasing temperature or increasing pressure. Compound 3 does not emit under ambient conditions but displays increasingly red-shifted luminescence upon cooling or compression. Compound 4 remains emissionless, consistent with the absence of intermolecular Au∙∙∙Au interactions. The largest pressure induced shift in emission is observed in 2 with a red shift of approximately 630 cm -1 per GPa between ambient and 3.80 GPa. The shifts in all the complexes can be correlated with changes in Au∙∙∙Au distance observed by diffraction.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2018

The Effect of Voltage Charging on the Transport Properties of Gold Nanotube Membranes

Porous membranes are typically used in chemical separations and in many electrochemical processes and devices. Research on the transport properties of a unique class of porous membranes that contain monodisperse gold nanotubes traversing the entire membrane thickness is reviewed here. These gold nanotubes can act as conduits for ionic and molecular transports through the membrane. Because the tubes are electronically conductive, they can be electrochemically charged by applying a voltage to the membrane. How this “voltage charging” works with the transport properties of gold nanotube membranes is the subject of this Review. Experiments demonstrating that voltage charging can be used to reversibly switch the membrane between ideally cation- and anion-transporting states are reviewed. Voltage charging can also be used to enhance the ionic conductivity of gold nanotube membranes. Finally, voltage charging to accomplish electroporation of living bacteria as they pass through gold nanotube membranes is reviewed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Extraction of gold, mercury, and lead with TEVA resin from HCl and HNO 3

The extraction behavior of 212 Pb, 197m Hg, and 194 Au on TEVA resin in HCl and HNO 3 solutions was studied with batch uptake, kinetics, and column studies. The uptake of mercury and gold was extremely high from HCl solutions, with maximum k’ >80,000 for both elements. The uptake of mercury was lower in HNO3 than HCl with a maximum k’ of ~ 8,000 in 0.02 M HNO 3 and decreasing uptake at higher concentrations of HNO3, which agrees well with previous work. The batch uptake of gold in HNO 3 was not measured, as it had been reported previously. The uptake of lead on TEVA resin in HCl was low with a maximum k’ of only ~ 90 in 1 M HCl. The uptake of lead in HNO 3 was negligible. The uptake kinetics of gold and mercury were characterized in HCl and HNO 3 solutions and high uptake was seen after ~ 60 s for both elements. Column separations of 212 Pb, 197m Hg, and 194 Au on TEVA resin from HCl and HNO 3 solutions are reported with high yields of mercury and lead, but with high losses of gold, which is retained on the resin. A rapid, high yield separation of 197m Hg from irradiated gold foils is presented with yields of ~ 100% for both elements and a total separation time of < 2 h.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗