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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Laser Ablation Generation of Antimony Selenide Clusters: Laser Desorption Ionization (LDI) Quadrupole Ion Trap Time of Flight Mass Spectrometry

The binary system Sb-Se was studied via laser ablation using antimony-selenium mixtures made from powdered elements in various ratios generating new Sb{sub m}Se{sub n} clusters. The results show that in addition to Sb{sub m}{sup +} (m = 1–8) and Se{sub n}{sup +} (n = 2–9) clusters, a series of Sb{sub m}Se{sub n}{sup +} clusters such as SbSe{sub 1–8}{sup +}, Sb{sub 2}Se{sub 1–6}{sup +}, Sb{sub 3}Se{sub 1–5}{sup +}, Sb{sub 4}Se{sub 1–3}{sup +}, and Sb{sub 5}Se{sub 1,2}{sup +} is generated. In addition, some low intensity oxidized clusters like Se{sub 6}O{sub 2}{sup +}, Se{sub 7}O{sub 2}{sup +}, and SbSe{sub 2-6}O{sub 5}{sup +} and partially hydroxylated clusters (SbSeO{sub 2}H{sub 7}{sup +}, SbSe{sub 5}O{sub 4}H{sup +}) are also formed. In total, 24 new antimony selenide clusters were generated. The knowledge gained can contribute to the elucidation of the structure of Sb{sub m}Se{sub n} glasses. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2023

A heat flux sensor leveraging the transverse Seebeck effect in elemental antimony

Certain configurations of anisotropic single crystal materials can generate a thermoelectric voltage orthogonal to an induced temperature gradient. This phenomenon is known as the Transverse Seebeck Effect (TSE) and can be leveraged to fabricate simple and robust heat flux sensors. Only a small number of materials have been considered as TSE-based transducers and, among these, few have been developed into sensors with ruggedization against chemical and mechanical degradation. Here, we report on the fabrication and characterization of a rugged TSE-based heat flux sensor using prismatic antimony single crystals. The heat flux sensor was tested under static and dynamic heating scenarios. The sensor has a linear responsivity of 16.8 µV/(W/cm2) to heat fluxes spanning more than two orders of magnitude and a time constant of 4.4 s. The sensor’s response to localized heating, probed with a laser scanning technique, validated that the transduction mechanism is primarily the TSE by ruling out a sizable contribution from the conventional Seebeck effect. Finite element analysis corroborated that components used in the sensor package are the primary determinants of the time constant and the decrement of the responsivity from its theoretical maximum. Design principles that may be applied to elicit a faster transient response or higher responsivity are proposed. Furthermore, the results establish single crystal antimony as a promising transducer material for heat flux measurement systems and demonstrate potential effects of ruggedization on sensor performance.

36 MATERIALS SCIENCE↗
DOE OSTI2019

The h –Sb x WO 3+2 x Oxygen Excess Antimony Tungsten Bronze

Here, we describe the previously unreported oxygen excess hexagonal antimony tungsten bronze with composition Sb 0.5 W 3 O 10 , in the following denoted as h –Sb x WO 3+2 x with x = 0.167, to demonstrate its analogy to classical A x WO 3 tungsten bronzes. This compound forms in a relatively narrow temperature range between 580 °C < T < 620 °C. It was obtained as a dark–blue polycrystalline powder, and as thin, needle–shaped, blue single crystals. h –Sb x WO 3+2 x crystallizes in the hexagonal space group P 6/ mmm with the cell parameters a=7.4369(4) Å and c=3.7800(2) Å. The antimony and excess oxygen occupy the hexagonal channels within the network of corner–sharing WO 6 octahedra. h –Sb x WO 3+2 x has a resistivity of ρ 300 K ≈1.28 mΩ cm at room temperature, with little if any temperature–dependence on cooling. DFT calculations on a simplified model for this compound find a metallic–like electronic structure with the Fermi level falling within rather flat bands, especially around the Γ point.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

A Damage Model for Degradation in the Electrodes of solid oxide fuel cells: Modeling the effects of sulfur and antimony in the anode

Over their designed lifetime, high temperature electrochemical devices, such as solid oxide fuel cells (SOFCs), can experience degradation in their electrochemical performance due to environmental conditions, operating conditions, contaminants, and other factors. Understanding the different degradation mechanisms in SOFCs and other electrochemical devices is essential to reducing performance degradation and increasing the lifetime of these devices. In this paper SOFC degradation mechanisms are discussed and a damage model is presented which describes performance degradation in SOFCs due to damage or degradation in the electrodes of the SOFC. A degradation classification scheme is presented that divides the various SOFC electrode degradation mechanisms into categories based on their physical effects on the SOFC. The application of the damage model and the classification method is applied to sulfur poisoning and antimony poisoning which occur in the anode of SOFCs. For sulfur poisoning the model is able to predict the degradation in SOFC performance based on the operating temperature and voltage of the fuel cell and the concentration of gaseous sulfur species in the anode. For antimony poisoning the effects of nickel removal from the anode matrix is investigated.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2015

Effect of indium and antimony doping in SnS single crystals

Highlights: • Single crystals growth of pure SnS, indium doped SnS and antimony doped SnS by direct vapour transport (DVT) technique. • Doping of In and Sb occurred in SnS single crystals by cation replacement. • The replacement mechanism ascertained by EDAX, XRD and substantiated by Raman spectra analysis. • Dopants concentration affects the optical energy bandgap. • Doping influences electrical transport properties. - Abstract: Single crystals of pure SnS, indium (In) doped SnS and antimony (Sb) doped SnS were grown by direct vapour transport (DVT) technique. Two doping concentrations of 5% and 15% each were employed for both In and Sb dopants. Thus in total five samples were studied viz., pure SnS (S1), 5% In doped SnS (S2), 15% In doped SnS (S3), 5% Sb doped SnS (S4) and 15% Sb doped SnS (S5). The grown single crystal samples were characterized by evaluating their surface microstructure, stoichiometric composition, crystal structure, Raman spectroscopy, optical and electrical transport properties using appropriate techniques. The d.c. electrical resistivity and thermoelectric power variations with temperature showed semiconducting and p-type nature of the as-grown single crystal samples. The room temperature Hall Effect measurements further substantiated the semiconducting and p-type nature of the as-grown single crystal samples. The obtained results are deliberated in detail.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Rh → Sb Interactions Supported by Tris(8-quinolyl)antimony Ligands

The study of ambiphilic systems combining L-type and Z-type ligands within the same construct has emerged as a field of active investigation, especially in the cases of ligands containing a group 13 element as a σ-acceptor for transition metals. (1) Parallel to these developments, several groups have investigated more atypical systems in which the Z-type ligand is a group 15 element. (2) Our contributions to this area have focused on the use of phosphinostibine ligands for the generation of transition metal complexes in which the antimony moiety acts as a Z-type ligand. (1d,3) We have shown that the magnitude of the resulting M → Sb interaction can be readily modulated by the oxidation state of the antimony atom (4) as well as its charge which can be manipulated by abstraction of anionic ligands. (5) Our work has also shown that these effects can be leveraged to enhance the catalytic properties of the transition metal center. (4,5) Some of the simplest systems that we have investigated are those resulting from the reaction of platinum dichloride with the bis- or tris-phosphinostibines ClSb(o-dppp) 2 and Sb(o-dppp) 3 , respectively (o-dppp = o-(Ph 2 P)C 6 H 4 ). These reactions proceed by oxidative insertion of the stibine into a Pt- Cl bond to produce complexes A and B, (6) respectively (Chart 1). Reasoning that the properties of these complexes may also be influenced by the nature of the L-type buttresses, we have now questioned whether stibines featuring nitrogen donor ligands could also display the redox noninnocence of their phosphine counterparts and support the formation of such complexes. Following up on some of our work with ambiphilic tellurium-quinoline ligands, (7) we now report on the reaction of tris-(8-quinolyl)stibines (8) toward (MeCN) 3 RhCl 3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Annealing effects on structural, electrical and optical properties of antimony-tinoxide thin films deposited by sol gel dip coating technique

Antimony-doped tin dioxide possess interesting physical and chemical properties. These properties have a wide range of applications such as catalysis and optoelectronic devices. In the present study, antimony-doped tin oxide (SnO2:Sb) thin films were deposited on the quartz substrates by sol-gel dip coating technique. The films were annealed at temperatures 350°C, 550°C and 850°C in air for 2 hours. The structure and surface morphologies were observed by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). XRD patterns shows tetragonal structure for the SnO2:Sb films annealed at different temperatures. Crystallite size increased from 6 to 14 nm as annealing temperature increased from 350°C to 850°C. SEM studies reveals crack free and smooth surface for all the films. The grains are found to be homogenously distributed for films annealed at higher temperature. The electrical conductivity of the films annealed at 350°C and 550°C decreased and increased for the films annealed at 850°C. The optical properties of the films were investigated in the UV-visible-NIR region (200-900 nm) using UV spectra. The transmittance of the films decreased for films annealed at higher temperature. The optical energy band gap values (4.13 eV-4.83 eV) increased with the increase in annealing temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Thermoelectric properties of antimony selenide hexagonal nanotubes

Antimony selenide (Sb 2 Se 3 ) is a material widely used in photodetectors and relatively new as a possible material for thermoelectric applications. Taking advantage of the new properties after nanoscale fabrication, this material shows great potential for the development of efficient low temperature thermoelectric devices. Here, for this paper, we study the synthesis, the crystal properties and the thermal and thermoelectric transport response of Sb 2 Se 3 hexagonal nanotubes (HNT) in the temperature range between 120 and 370 K. HNT have a moderate electrical conductivity ~10 2 S m -1 while maintaining a reasonable Seebeck coefficient ~430 μV K -1 at 370 K. The electrical conductivity in Sb 2 Se 3 HNT is about 5 orders of magnitude larger and its thermal conductivity one half of what is found in bulk. Moreover, the calculated figure of merit (ZT) at room temperature is the largest value reported in antimony selenide 1D structures.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Antimony segregation in stressed SiGe heterostructures grown by molecular beam epitaxy

The effects of the growth temperature, composition, and elastic strains in separate layers on the segregation of antimony are studied experimentally for stressed SiGe structures grown by molecular beam epitaxy. It is established that the growth conditions and parameters of the structures exert an interrelated influence on the segregation of Sb: the degree of the influence of the composition and elastic stresses in the SiGe layers on Sb segregation depends on the growth temperature. It is shown that usage of a method previously proposed by us for the selective doping of silicon structures with consideration for the obtained dependences of Sb segregation on the growth conditions and parameters of the SiGe layers makes it possible to form SiGe structures selectively doped with antimony.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dielectric Losses and Charge Transfer in Antimony-Doped TlGaS{sub 2} Single Crystal

Effect of semimetallic antimony (0.5 mol % Sb) on the dielectric properties and ac-conductivity of TlGaS{sub 2}-based single crystals grown by the Bridgman–Stockbarger method has been studied. The experimental results on the frequency dispersion of dielectric coefficients and the conductivity of TlGa{sub 0.995}Sb{sub 0.005}S{sub 2} single crystals allowed the revealing of the dielectric loss nature, the charge transfer mechanism, and the estimation of the parameters of the states localized in the energy gap. The antimony-doping of the TlGaS{sub 2} single crystal leads to an increase in the density of states near the Fermi level and a decrease in the average time and average distance of hopes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Reaction of Antimony-Uranium Composite Oxide in the Chlorination Treatment of Waste Catalyst - 13521

The effect of oxygen gas concentration on the chlorination treatment of antimony-uranium composite oxide catalyst waste was investigated by adding different concentrations of oxygen at 0-6 vol% to its chlorination agent of 0.6 or 6 vol% hydrogen chloride gas at 1173 K. The addition of oxygen tended to prevent the chlorination of antimony in the oxide. When 6 vol% hydrogen chloride gas was used, the addition of oxygen up to 0.1 vol% could convert the uranium contained in the catalyst to U{sub 3}O{sub 8} without any significant decrease in the reaction rate compared to that of the treatment without oxygen. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

High Angle Remediation Antimony, Mercury, and Pu-239/240 Contaminated Soil at LANL near Los Alamos Town Site - 18579

The Manhattan Project and early Cold War era operations at Los Alamos National Laboratory (LANL) left behind soil contaminated with antimony, mercury, and Pu-239/240. TerranearPMC (TPMC) successfully completed a phased three-year high-angle legacy cleanup project to excavate contaminated soil from a steep, difficult-to-access canyon wall in the Upper Los Alamos Canyon Aggregate Area bordering Los Alamos town site. The first and third phases of the project (years 2015 and 2017) utilized a Menzi Muck (spider excavator) in concert with a 275 US ton telescoping crane to remove ∼158 cubic yards (cy) of mercury-contaminated rock and soil (i.e. media) from one solid waste management unit (SWMU) in 2015; and ∼70 cy of antimony contaminated media, and ∼65 cy of collocated mercury and Pu-239/240 contaminated media from two SWMUs in 2017. All soil excavated from the site was containerized in soft-sided 1.0 cy, 1.77 cy, and 3.5 cy IP-1 containers and shipped to an approved, licensed, off-site disposal facility. The crane was also used to move the spider excavator, field personnel, tools, the packaged waste, and restoration materials into and out of the canyon. In 2016, conventional but miniaturized excavation equipment was used to remove about 133 cy of Pu-239/240 contaminated media from four SWMUs west of both the 2015 and 2017 excavations. A total of 398 soil screening, waste composite, characterization/bounding, and confirmation samples were collected during the project. Media that was left in place after the excavation was sampled to confirm that human health concerns and environmental risk issues had been mitigated. This proven technical approach was the preferred method for cleaning up ∼426 cy of contaminated media from steep, difficult-to-access legacy waste sites within the Upper Los Alamos Canyon Aggregate Area between 2015 and 2017. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Preparation and Characterization of Antimony and Arsenic Tricyanide and Their 2,2′‐Bipyridine Adducts

Abstract The arsenic(III) and antimony(III) cyanides M(CN) 3 (M=As, Sb) have been prepared in quantitative yields from the corresponding trifluorides through fluoride–cyanide exchange with Me 3 SiCN in acetonitrile. When the reaction was carried out in the presence of one equivalent of 2,2′‐bipyridine, the adducts [M(CN) 3 ⋅ (2,2′‐bipy)] were obtained. The crystal structures of As(CN) 3 , [As(CN) 3 ⋅ (2,2′‐bipy)] and [Sb(CN) 3 ⋅ (2,2′‐bipy)] were determined and are surprisingly different. As(CN) 3 possesses a polymeric three‐dimensional structure, [As(CN) 3 ⋅ (2,2′‐bipy)] exhibits a two‐dimensional sheet structure, and [Sb(CN) 3 ⋅ (2,2′‐bipy)] has a chain structure, and none of the structures resembles those found for the corresponding arsenic and antimony triazides.

Deokar, Piyush↗
DOE OSTI2026

Kinetic control of phase evolution and defect-mediated recombination in AACVD-grown copper antimony sulphide thin films

Copper antimony sulphide (CAS) is a multinary chalcogenide semiconductor in which small deviations from stoichiometry can drive phase competition and strong defect-mediated modulation of optoelectronic properties. However, the systematic roles of copper precursor fraction and deposition time in governing phase evolution, off-stoichiometry, and recombination dynamics in aerosol-assisted chemical vapour deposition (AACVD)-grown undoped CAS thin films remain insufficiently understood. In this work, undoped CAS thin films were deposited by AACVD using Cu(dedtc)2 and Sb(dedtc)3 single-source precursors at 550 °C and a carrier gas flow rate of 150 sccm, while the Cu(dedtc)2 mole fraction (x = 0.15 – 0.55) and deposition time (1 – 2 hours) were systematically varied to probe how growth kinetics influence phase composition, microstructure, and defect-mediated optical properties without post-deposition annealing or extrinsic doping. Increasing copper precursor content drives phase evolution toward tetrahedrite-dominant CAS films at intermediate Cu(dedtc)2 mole fractions, with the film deposited at x = 0.35 exhibiting the strongest tetrahedrite character within the parameter space examined. The films are also copper-rich, antimony-poor, and sulphur-deficient, consistent with off-stoichiometric growth and intrinsic defect formation, plausibly including copper interstitials, Cu-on-Sb antisites, and sulphur vacancies. These growth-dependent compositional deviations are accompanied by tunable indirect optical bandgaps of approximately 1.60 – 2.18 eV and weak visible photoluminescence governed by defect-mediated recombination. Time-resolved photoluminescence reveals bi-exponential decay behaviour with lifetimes of approximately 0.1 – 3.6 ns, with emission dominated by slower donor–acceptor pair recombination and a smaller contribution from faster trap-assisted pathways. Collectively, these results establish an explicit kinetic process–structure–defect–property relationship for AACVD-grown CAS thin films and provide a growth–structure–property framework relevant to future optimization of CAS-based optoelectronic and energy materials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ultrathin high- κ antimony oxide single crystals

Ultrathin oxides have been reported to possess excellent properties in electronic, magnetic, optical, and catalytic fields. However, the current and primary approaches toward the preparation of ultrathin oxides are only applicable to amorphous or polycrystalline oxide nanosheets or films. Here, we successfully synthesize high-quality ultrathin antimony oxide single crystals via a substrate-buffer-controlled chemical vapor deposition strategy. The as-obtained ultrathin antimony oxide single crystals exhibit high dielectric constant (~100) and large breakdown voltage (~5.7 GVm -1 ). Such a strategy can also be utilized to fabricate other ultrathin oxides, opening up an avenue in broadening the applicaitons of ultrathin oxides in many emerging fields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Metal ion dopant-induced famatinite to chalcostibite phase transformation of copper antimony sulphide colloidal nanostructures: effect on photophysical and pseudocapacitance properties

Here, the strategic doping of transition metal ions into copper antimony sulphide (CAS) semiconducting nanostructures can significantly influence their photophysical and pseudocapacitive properties, for which there are few reports and therefore is the focus of this study. Accordingly, highly crystalline metal ion (Mn 2+ , Fe 2+ , Co 2+ , Ni 2+ and Zn 2+ ) doped off-stoichiometric copper rich/poor, antimony-rich/poor, and sulphur-poor CAS nanostructures (10–23 nm) were grown via colloidal (hot-injection) synthesis using metal diethyldithiocarbamate precursors. Importantly, metal ion doping significantly influences the structure and composition of the off-stoichiometric CAS nanostructures. Data from powder X-ray diffraction, Raman spectroscopy, high-resolution scanning/transmission electron microscopy, and energy dispersive X-ray spectroscopy confirm that the heavier metal ion dopants induce a novel phase transformation from famatinite (fCAS) to chalcostibite (cCAS) nanostructures. The influence of the metal ion dopants is also observed in the optical properties of as-synthesized nanostructures. This involves blue-shifted ultraviolet-visible absorption, reduced Urbach tailing, and tunable bandgaps between 2.17 and 2.38 eV. Also, the doped nanostructures display broad visible-near infrared photoluminescence via a triple radiative pathway with relatively short decay lifetimes between 0.2 and 6.1 ns. This is mediated by electronic transitions involving intrinsic (copper/antimony/sulphur interstitial) and extrinsic (metal ion interstitial) defect states. Additionally, electrodes prepared from Mn 2+ -doped fCAS nanostructures show enhanced pseudocapacitance via Na+ surface adsorption and intercalation relative to undoped fCAS electrodes, while Zn 2+ -doped cCAS electrodes exhibit pseudocapacitance via a combination of Na+ surface adsorption, intercalation, and redox reactions. These electrodes exhibit reduced charge transfer resistance, improved electronic conductivity and notably enhanced specific capacitance (∼222 F g −1 ), and charge transport, as measured in 1 M Na 2 SO 4 electrolyte via cyclic voltammetry and electrochemical impedance spectroscopy. To this end, the discovery of the metal ion-induced phase transformation presents a new avenue for optimizing the functional properties of fCAS and cCAS nanostructures, highlighting the critical role of metal ion-related defects in controlling the optical and electrochemical properties, towards potential solar absorption and energy storage applications.

25 ENERGY STORAGE↗
DOE OSTI2019

Identification of Phase Transitions and Metastability in Dynamically Compressed Antimony Using Ultrafast X-Ray Diffraction

Ultrafast x-ray diffraction at the LCLS x-ray free electron laser has been used to resolve the structural behavior of antimony under shock compression to 59 GPa. Antimony is seen to transform to the incommensurate, host-guest phase Sb-II at ~11 GPa, which forms on nanosecond timescales with ordered guest-atom chains. The high-pressure bcc phase Sb-III is observed above ~15 GPa, some 8 GPa lower than in static compression studies, and mixed Sb-III/liquid diffraction are obtained between 38 and 59 GPa. An additional phase which does not exist under static compression, Sb–I', is also observed between 8 and 12 GPa, beyond the normal stability field of Sb-I, and resembles Sb-I with a resolved Peierls distortion. In conclusion, the incommensurate Sb-II high-pressure phase can be recovered metastably on release to ambient pressure, where it is stable for more than 10 ns.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗