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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Tin Nitride Atomic Layer Deposition Using N2H4

There is substantial lag in the development of atomic layer deposition (ALD) processes for nitrides compared to the high-quality, conformal oxides for which ALD has become the standard. A major factor in this disparity is the ready availability of highly reactive oxygen sources (mainly H2O, O2, and H2O2). High-energy nitrogen precursors are similarly required for the efficient incorporation of nitrogen in a film. Ammonia has often been used in conjunction with metal chlorides but requires relatively high temperatures for thermal ALD. Plasma-enhanced ALD can utilize molecular nitrogen as a precursor but can reduce film conformality on complex supports and damage the underlying substrate. Hydrazine (N2H4) is an alternative precursor which has been rarely explored for the fabrication of nitrides in ALD, but which is experiencing a surge in popularity due to its high reactivity, which enables the deposition of nitrides as-yet undemonstrated by ALD.(1) The added reactivity and volatility of liquid hydrazine may enable new reaction mechanisms, lower deposition temperatures, and conformality for high aspect ratio applications. Sn3N4 is a metastable semiconductor which shares a crystal structure with its analog, Si3N4; unlike Si3N4, Sn3N4 has only recently been grown by ALD,(2) being synthesized much more often through reactive sputtering.(3) As a binary, Sn3N4 has applications as a battery anode material, for photoelectrochemistry, and optoelectronic devices. We will report progress on the deposition of SnxNy films from tetrakis(dimethylamido) tin (TDMASn) and N2H4. Growth per cycle of this material (determined by x-ray reflectivity) is 0.4 A at 200 C, similar to the sole report of Sn3N4 from PE-ALD,(2) despite films being substantially Sn-rich. Identification of ALD growth window and self-limiting deposition characteristics are underway; initial testing indicates a competing chemical vapor deposition process which can be eliminated with adequate tuning of pulse/purge characteristics. A comparison of film conductivity and optical absorption at different growth temperatures will be presented. General issues of N2H4 purity and routes to prevent or control oxynitride formation will be discussed. (1) Du, L., et al. The First Atomic Layer Deposition Process for FexN Films. Chem. Comm., 2019, ASAP. DOI: 10.1039/C8CC10175B. (2) Stewart, D. M., et al. Tin Oxynitride Anodes by Atomic Layer Deposition for Solid-State Batteries. Chem. Mater. 2018, 30, 2526-34. (3) Caskey, C. M., et al. Semiconducting Properties of Spinel Tin Nitride and Other IV3N4 Polymorphs. J. Mater. Chem. C 2015, 3, 1389-96.

14 SOLAR ENERGY↗
DOE OSTI2016

One-pot synthesis of tin-borophosphate-carbon composites as anode materials for Li-ion batteries

Sn{sub x}(Ca{sub 0.05}B{sub 0.975}P{sub 0.975}O{sub 3.95}){sub 1−x}/C composites as anode material for Li-ion batteries, with x=0.83 and x=0.71 were synthesized by a facile route including cellulose as carbon source. The composites were characterized by X-ray diffraction, scanning electron microscopy, Raman spectroscopy and {sup 119}Sn Mössbauer spectroscopy. In the latter case, different tin phases were found in the composite including the Sn{sup II}-based amorphous interface between metallic tin and borophosphate particles that improves the dispersion of the active species. The best electrochemical performances were obtained for x=0.71 that were further improved by ball-milled the composite with a small amount of carbon black. - Graphical abstract: {sup 119}Sn Mössbauer spectra of Sn{sub x}(Ca{sub 0.05}B{sub 0.975}P{sub 0.975}O{sub 3.95}){sub 1−x}/C composites with x=0.83 (a) and x=0.71 (b).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

An in situ x-ray photoelectron spectroscopy study of the initial stages of rf magnetron sputter deposition of indium tin oxide on p-type Si substrate

The interface between indium tin oxide and p-type silicon is studied by in situ X-ray photoelectron spectroscopy (XPS). This is done by performing XPS without breaking vacuum after deposition of ultrathin layers in sequences. Elemental tin and indium are shown to be present at the interface, both after 2 and 10 s of deposition. In addition, the silicon oxide layer at the interface is shown to be composed of mainly silicon suboxides rather than silicon dioxide.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Hydrogen plasma treatment for improved conductivity in amorphous aluminum doped zinc tin oxide thin films

Improving the conductivity of earth-abundant transparent conductive oxides (TCOs) remains an important challenge that will facilitate the replacement of indium-based TCOs. Here, we show that a hydrogen (H{sub 2})-plasma post-deposition treatment improves the conductivity of amorphous aluminum-doped zinc tin oxide while retaining its low optical absorption. We found that the H{sub 2}-plasma treatment performed at a substrate temperature of 50 °C reduces the resistivity of the films by 57% and increases the absorptance by only 2%. Additionally, the low substrate temperature delays the known formation of tin particles with the plasma and it allows the application of the process to temperature-sensitive substrates.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Direct transparent electrode patterning on layered GaN substrate by screen printing of indium tin oxide nanoparticle ink for Eu-doped GaN red light-emitting diode

Transparent electrodes were formed on Eu-doped GaN-based red-light-emitting diode (GaN:Eu LED) substrates by the screen printing of indium tin oxide nanoparticle (ITO np) inks as a wet process. The ITO nps with a mean diameter of 25 nm were synthesized by the controlled thermolysis of a mixture of indium complexes and tin complexes. After the direct screen printing of ITO np inks on GaN:Eu LED substrates and sintering at 850 °C for 10 min under atmospheric conditions, the resistivity of the ITO film was 5.2 mΩ cm. The fabricated LED up to 3 mm square surface emitted red light when the on-voltage was exceeded.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Isotope tracer investigation and ab-initio simulation of anisotropic hydrogen transport and possible multi-hydrogen centers in tin dioxide

Hydrogen as an impurity in single crystals of tin dioxide was investigated through diffusivity and vibrational-mode analyses performed using isotope tracers and density functional theory calculations. It was found that hydrogen diffusion along the 〈001〉 axis is very fast, even at relatively low temperatures (400 °C), but is considerably slower within the (001) plane. Using transitional state calculations, this diffusion behavior was determined to be the result of anisotropy in the migration barrier for interstitial hydrogen (H{sub i}). In addition, the two distinct vibrational modes observed in the optical spectrum were identified as the O-H stretching modes of Hi and the substitutional hydrogen at the tin sites.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Dispersive optical-model potential for protons in 100 ⩽ A ⩽ 132 even–even tin isotopes

Data on single-particle energies, differential elastic-scattering cross sections, and total cross sections for proton-induced reactions on stable tin isotopes were analyzed on the basis of the dispersive optical model. Good agreement with experimental data was obtained by setting the parameters of the dispersive optical potential to values averaged over the tin isotopic chain and by assuming that the dependence of surface absorption on the neutron–proton asymmetry is close to a traditional dependence. Predictive calculations for single-particle proton spectra and total reaction cross sections were performed for the doubly magic isotopes {sup 100,132}Sn. The calculated values of the energy gap between the 1h{sub 11/2}–1g{sub 7/2} and 1g{sub 7/2}–2d{sub 5/2} states were found to be in good agreement with the results of calculations performed with allowance for the tensor component of the effective nucleon–nucleon interaction.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2016

On the electrical and optical properties of oxide nanolayers produced by the thermal oxidation of metal tin

Thin SnO{sub 2–x} layers, 30 nm in thickness, are produced by the thermal oxidation of metal tin nanolayers at a temperature of 450–750°C. The electrical and optical properties of the layers are studied. During the thermal oxidation of tin nanolayers, an unsteady variation in their conductivity is observed. For the oxide films produced at 450 and 550°C, an absorption band at 340 nm (3.65 eV) is detected in the optical spectra. The conductivity-activation energy is determined for samples oxidized to different degrees. On the basis of experimental data and the data reported in publications, an oxidation mechanism controlling the properties of Sn nanolayers is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2015

3D Scaffolded Nickel-Tin Li-Ion Anodes with Enhanced Cyclability

A 3D mechanically stable scaffold is shown to accommodate the volume change of a high-specific-capacity nickel–tin nanocomposite during operation as a Li-ion battery anode. Here, the nickel–tin anode is supported by an electrochemically inactive conductive scaffold with an engineered free volume and controlled characteristic dimensions, which engender the electrode with significantly improved cyclability.

25 ENERGY STORAGE↗
DOE OSTI2024

A Lead‐Free Ferroelectric 2D Dion–Jacobson Tin Iodide Perovskite

2D hybrid organic–inorganic halide perovskites emerge as a new class of 2D semiconductors with the potential to combine excellent optoelectronic properties with symmetry-enabled properties such as ferroelectricity. Although many lead-based ferroelectric 2D halide perovskites are reported, there is yet to be a conclusive report of ferroelectricity in tin-based 2D perovskites. Here, the structures and properties of a new series of 2D Dion–Jacobson (DJ) Sn perovskites: (4AMP)SnI 4 , (4AMP)(MA)Sn 2 I 7 , and (4AMP)(FA)Sn 2 I 7 (4AMP = 4-(aminomethyl)piperidinium, MA = methylammonium, and FA = formamidinium), are reported. Structural characterization reveals that (4AMP)SnI 4 is polar with in-plane spontaneous polarization whereas (4AMP)(MA)Sn 2 I 7 and (4AMP)(FA)Sn 2 I 7 are centrosymmetric. Further, (4AMP)SnI 4 displays second harmonic generation (SHG) and polarization-electric field hysteresis measurements confirm it is ferroelectric with a spontaneous polarization of 10.0 µC cm −2 at room temperature. (4AMP)SnI 4 transitions into a centrosymmetric structure above 367 K. As the first direct experimental observation of the spontaneous ferroelectric polarization of a Sn-based 2D hybrid perovskite, this work opens up environmentally friendly 2D tin halide perovskites for ferroelectricity and other physical property studies.

2D↗
DOE OSTI2019

Microstructural Characteristics and Mechanical Properties of Friction-Stir-Welded CuSn6 Tin Bronze

Tin bronze is widely applied in various industries for its excellent wear and corrosion resistance. Friction stir welding is a solid-state welding process, which generates less heat and avoids the melting-related defects. CuSn6 tin bronze plates of 4 mm in thickness were friction-stir-welded at welding speeds ranging from 50 to 150 mm/min under a constant rotation speed. The microstructural and mechanical properties of joints were investigated. The microstructure of the stir zone consists of refined equiaxed grains. The grain size decreased from top to bottom of the welds. The mean grain size is increased with increasing welding speed. The largest strength and elongation of welded joints were both obtained at the welding speed of 100 mm/min. During tensile test, all of the joints were fractured at the heat affected zone of retreating side with typical plastic fracture feature, since the grains were coarsened by welding heat.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Selective recovery of pure copper nanopowder from indium-tin-oxide etching wastewater by various wet chemical reduction process: Understanding their chemistry and comparisons of sustainable valorization processes

Sustainable valorization processes for selective recovery of pure copper nanopowder from Indium-Tin-Oxide (ITO) etching wastewater by various wet chemical reduction processes, their chemistry has been investigated and compared. After the indium recovery by solvent extraction from ITO etching wastewater, the same is also an environmental challenge, needs to be treated before disposal. After the indium recovery, ITO etching wastewater contains 6.11 kg/m{sup 3} of copper and 1.35 kg/m{sup 3} of aluminum, pH of the solution is very low converging to 0 and contain a significant amount of chlorine in the media. In this study, pure copper nanopowder was recovered using various reducing reagents by wet chemical reduction and characterized. Different reducing agents like a metallic, an inorganic acid and an organic acid were used to understand reduction behavior of copper in the presence of aluminum in a strong chloride medium of the ITO etching wastewater. The effect of a polymer surfactant Polyvinylpyrrolidone (PVP), which was included to prevent aggregation, to provide dispersion stability and control the size of copper nanopowder was investigated and compared. The developed copper nanopowder recovery techniques are techno-economical feasible processes for commercial production of copper nanopowder in the range of 100–500 nm size from the reported facilities through a one-pot synthesis. By all the process reported pure copper nanopowder can be recovered with>99% efficiency. After the copper recovery, copper concentration in the wastewater reduced to acceptable limit recommended by WHO for wastewater disposal. The process is not only beneficial for recycling of copper, but also helps to address environment challenged posed by ITO etching wastewater. From a complex wastewater, synthesis of pure copper nanopowder using various wet chemical reduction route and their comparison is the novelty of this recovery process. - Highlights: • From the Indium-Tin-Oxide etching wastewater, copper nanopowder was synthesized. • Solution chemistry of ITO etching wastewater is addressed. • A techno-economical feasible, environment friendly and occupational safe process. • Brings back the material to production stream and address the circular economy. • A cradle to cradle technology management lowers the futuristic carbon economy.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

X-ray induced synthesis of beta tin (β-Sn)

The destabilization of molecular structures via hard X-rays has been previously utilized to synthesize novel compounds. Here, in this study, we report that the monochromatic X-ray induced decomposition of tin(II) oxalate (SnC 2 O 4 ) at ambient and 0.6 GPa pressures lead to the formation of beta tin (β-Sn). At 1 GPa, only the degradation of SnC 2 O 4 crystal structure is observed without any indication of β-Sn at the end of irradiation. The maximum transformation yield is achieved at 0.6 GPa suggesting the critical role of intermolecular distance in X-ray induced synthesis of β-Sn. Moreover, a modified Avrami equation is utilized to describe the kinetics and geometry of structural synthesis at ambient and 0.6 GPa. The obtained results demonstrate that X-ray irradiation can induce photochemical synthetic pathways different from conventional methods (e.g., high pressure, temperature, stoichiometric mixing) and that high pressure (HP) can be considered a tool to control X-ray induced photochemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

An alkaline tin(II) halide compound Na{sub 3}Sn{sub 2}F{sub 6}Cl: Synthesis, structure, and characterization

A new alkali tin(II) halide compound, Na{sub 3}Sn{sub 2}F{sub 6}Cl, is synthesized by hydrothermal method. This compound crystallizes trigonally in space group of R-3c (167), and processes a zero-dimensional (0D) structure consisted of Na{sup +} cations, Cl{sup −} anions and the isolated [SnF{sub 3}]{sup -} trigonal pyramids in which the stereochemically active 5s{sup 2} lone pair electrons are attached to the Sn{sup 2+} cations. Interestingly, the [SnF{sub 3}]{sup −} trigonal pyramids are parallel arranged in the a-b plane, while oppositely arranged in line with rotation along the c- axis. Moreover, the energy bandgap, thermal stability and electronic structure of Na{sub 3}Sn{sub 2}F{sub 6}Cl are characterized and the results reveal that this compound has and indirect bandgap of 3.88 eV and is stable under 270 °C. - Graphical abstract: A zero-dimensional alkaline tin halide compound, Na{sub 3}Sn{sub 2}F{sub 6}Cl, is synthesized by hydrothermal method. Interestingly, both the anions and cations coordinating polyhedra exhibit order arranged with the [SnF{sub 3}]{sup -} trigonal pyramids rotating along the c- axis.

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

Metallography and microstructure interpretation of some archaeological tin bronze vessels from Iran

Archaeological excavations in western Iran have recently revealed a significant Luristan Bronzes collection from Sangtarashan archaeological site. The site and its bronze collection are dated to Iron Age II/III of western Iran (10th–7th century BC) according to archaeological research. Alloy composition, microstructure and manufacturing technique of some sheet metal vessels are determined to reveal metallurgical processes in western Iran in the first millennium BC. Experimental analyses were carried out using Scanning Electron Microscopy–Energy Dispersive X-ray Spectroscopy and Optical Microscopy/Metallography methods. The results allowed reconstructing the manufacturing process of bronze vessels in Luristan. It proved that the samples have been manufactured with a binary copper–tin alloy with a variable tin content that may relates to the application of an uncontrolled procedure to make bronze alloy (e.g. co-smelting or cementation). The presence of elongated copper sulphide inclusions showed probable use of copper sulphide ores for metal production and smelting. Based on metallographic studies, a cycle of cold working and annealing was used to shape the bronze vessels. - Highlights: • Sangtarashan vessels are made by variable Cu-Sn alloys with some impurities. • Various compositions occurred due to applying uncontrolled smelting methods. • The microstructure represents thermo-mechanical process to shape bronze vessels. • In one case, the annealing didn’t remove the eutectoid remaining from casting. • The characteristics of the bronzes are similar to other Iron Age Luristan Bronzes.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microstructural, electrical and optical properties of indium tin oxide (ITO) nanoparticles synthesized by co-precipitation method

Highlights: Black-Right-Pointing-Pointer The grain size of the ITO is decreased from 28.7 to 9.0 nm by increasing Sn dopant. Black-Right-Pointing-Pointer The strain values increased with the incorporation of Sn in In{sub 2}O{sub 3} host lattice. Black-Right-Pointing-Pointer The lower resistivity of 4.9 {Omega} cm is obtained for 10 at.% Sn doped ITO. Black-Right-Pointing-Pointer The band gap varies from 3.62 to 3.89 eV with dopant concentration of Sn. -- Abstract: In the present study, the synthesis of Tin doped indium oxide (ITO) nanopowder at different compositions (In/Sn = 0, 5, 10, 15 at %) was carried out by co-precipitation method. The decomposition of precipitated indium tin acetylacetonate precursor to form In{sub 2}O{sub 3}-SnO{sub 2} (Sn{sub 1-x}In{sub x}O{sub 2}) at 400 Degree-Sign C was confirmed by the thermal and FTIR studies. The changes in strain and grain size of the synthesized particle with respect to dopant concentration were determined from the X-ray diffraction (XRD) analysis. Transmission electron microscopy (TEM) images support to confirm the grain size. The optical properties on ITO nanoparticles were analyzed with UV-visible spectroscopy, and band gap was found to vary from 3.62 to 3.89 eV with Sn dopant concentration. This variation was ascribed to the quantum confinement effect.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Low-temperature sintering behavior of nanocrystalline indium tin oxide prepared from polymer-containing sols

Highlights: Black-Right-Pointing-Pointer The synthesis of ITO powders and thin films from PVP-containing sols is presented. Black-Right-Pointing-Pointer The nano- and microstructures of ITO are more compact when PVP is used. Black-Right-Pointing-Pointer PVP acts both as a steric stabilizer of the sol and as a pre-sintering agent. Black-Right-Pointing-Pointer The PVP-induced enhanced sintering results in ITO with lower electrical resistance. Black-Right-Pointing-Pointer The surface composition of the ITO films is independent of the initial PVP content. -- Abstract: Indium tin hydroxide (ITH) xerogel powders and thin films with different polyvinylpyrrolidone (PVP) contents (0-22%, w/w) were prepared by a classical sol-gel method. To obtain nanocrystalline indium tin oxide (ITO), the ITH xerogels were calcined at 550 Degree-Sign C. The effect of the initial polymer content on the structure of the ITO powders was studied by means of N{sub 2}-sorption measurements, small-angle X-ray scattering (SAXS), transmission and scanning electron microscopy. The N{sub 2}-sorption measurements revealed that the ITO powders obtained contained micropores and both their porosity and specific surface area decreased with increasing PVP content of the ITH xerogels. The SAXS measurements confirmed the enhanced sintering of the particles in the presence of PVP. The calculated mass fractal dimensions of the ITO powders increased significantly, indicating a significant compaction in structure. The pre-sintered structure could be achieved at relatively low temperature, which induced a significant decreasing (three orders of magnitude) in the electrical resistance of the ITO films.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Optically active polyurethane@indium tin oxide nanocomposite: Preparation, characterization and study of infrared emissivity

Highlights: ► Silane coupling agent of KH550 was used to connect the ITO and polyurethanes. ► Infrared emissivity values of the hybrids were compared and analyzed. ► Interfacial synergistic action and orderly secondary structure were the key factors. -- Abstract: Optically active polyurethane@indium tin oxide and racemic polyurethane@indium tin oxide nanocomposites (LPU@ITO and RPU@ITO) were prepared by grafting the organics onto the surfaces of modified ITO nanoparticles. LPU@ITO and RPU@ITO composites based on the chiral and racemic tyrosine were characterized by FT-IR, UV–vis spectroscopy, X-ray diffraction (XRD), SEM, TEM, and thermogravimetric analysis (TGA), and the infrared emissivity values (8–14 μm) were investigated in addition. The results indicated that the polyurethanes had been successfully grafted onto the surfaces of ITO without destroying the crystalline structure. Both composites possessed the lower infrared emissivity values than the bare ITO nanoparticles, which indicated that the interfacial interaction had great effect on the infrared emissivity. Furthermore, LPU@ITO based on the optically active polyurethane had the virtue of regular secondary structure and more interfacial synergistic actions between organics and inorganics, thus it exhibited lower infrared emissivity value than RPU@ITO based on the racemic polyurethane.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗