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At least 199 records · Page 11

Characterization of Tri-lab β-Tin (Sn)

This report documents details of the microstructure and mechanical properties of -tin (Sn), that is used in the Tri-lab (Los Alamos National Laboratory (LANL), Lawrence Livermore National Laboratory (LLNL), Sandia National Laboratories (SNL)) collaboration project on Multi-phase Tin Strength. We report microstructural features detailing the crystallographic texture and grain morphology of as-received -tin from electron back scatter diffraction (EBSD). Temperature and strain rate dependent mechanical behavior was investigated by multiple compression tests at temperatures of 200K to 400K and strain rates of 0.0001 /s to 100 /s. Tri-lab tin showed significant temperature and strain rate dependent strength with no significant plastic anisotropy. A sample to sample material variation was observed from duplicate compression tests and texture measurements. Compression data was used to calibrate model parameters for temperature and rate dependent strength models, Johnson-Cook (JC), Zerilli-Armstrong (ZA) and Preston-Tonks-Wallace (PTW) strength models.

36 MATERIALS SCIENCE↗

Terrestrial growth of lead-tin-telluride by techniques related to low G growth

A modified Bridgman-Stockbarger furnace was constructed for a study of the solidification of silver, germanium and lead-tin-telluride. The melt-solid interface position with respect to the furnace and its temperature profile was determined by measuring the discontinuity in the slope of temperature as a function of position in the melt and in the solid. The results show that the interface position of the semiconductors germanium and lead-tin-telluride was essentially constant with respect to the furnace and hence the growth rate was constant and equal to the sample translation rate of 0.046 cm/min and 0.178 cm/min in each case. The metal, silver, on the other hand showed a continuous interface migration toward the hot zone of the furnace and always exhibited a growth rate which was higher than the ampoule translation rate. The K sub L/K sub S ratio of lead-tin-telluride was determined to be 2.33 + or - 0.06 where K sub L,S denotes the thermal conductivity of the liquid, solid respectively. The value of K sub L was calculated to be about 0.054 Watt 0.1 cm 0.1 K. The diffusion boundary layer thickness was calculated for lead-tin-telluride to be about 0.05 cm using a liquid diffusivity of .00007 sq cm/sec.

Jesser, W. A.↗

Infrared emission spectrophotometric study of the changes produced by TiN coating of metal surfaces in an operating EHD contact

Infrared emission spectra and related measurements were obtained from an operating ball/plate elastohydrodynamic (EHD) sliding contact under a variety of operating conditions. In order to be able to compare the effect of the ball surface, some of the balls were coated with a thin layer of titanium nitride (TiN) by vapor deposition. Polyphenyl ether (5P4E) was used as lubricant and 1 percent of 1,1,2-trichloroethane (TCE) as a surface-probing additive. TiN is chemically inert and its thermal conductivity is lower than that of steel. Therefore, the overall temperatures with TiN coated balls were higher. Nevertheless, no scuffing was observed with the coated balls under conditions giving rise to scuffing with the uncoated balls. Tractions were lower with the TiN coated balls and always when TCE was added to the 5P4E. These findings were found to be inversely related to the degree of polarization of the spectral emission bands. The intensity and the dichrosim of these bands were related to shear rates and inlet conditions of the EHD contact.

Keller, L. E.↗

A review of tin oxide-based catalytic systems: Preparation, characterization and catalytic behavior

This paper reviews the important aspects of the preparation, characterization and catalytic behavior of tin oxide-based catalytic systems including doped tin oxide, mixed oxides which contain tin oxide, Pt supported on tin oxide and Pt/Sn supported on alumina. These systems have a broad range of applications and are continually increasing in importance. However, due to their complex nature, much remains to be understood concerning how they function catalytically.

Hoflund, Gar B.↗

Process for making a noble metal on tin oxide catalyst

A quantity of reagent grade tin metal or compound, chloride-free, and high-surface-area silica spheres are placed in deionized water, followed by deaerating the mixture by boiling and adding an oxidizing agent, such as nitric acid. The nitric acid oxidizes the tin to metastannic acid which coats the spheres because the acid is absorbed on the substrate. The metastannic acid becomes tin oxide upon drying and calcining. The tin-oxide coated silica spheres are then placed in water and boiled. A chloride-free precious metal compound in aqueous solution is then added to the mixture containing the spheres, and the precious metal compound is reduced to a precious metal by use of a suitable reducing agent such as formic acid. Very beneficial results were obtained using the precious metal compound tetraammine platinum(II) hydroxide.

Upchurch, Billy T.↗

Effect of pretreatment on a platinized tin oxide catalyst used for low-temperature CO-oxidation

A commercial platinized tin oxide catalyst used for low-temperature CO oxidation has been characterized using ion scattering spectroscopy (ISS), Auger electron spectroscopy (AES) and Electron Spectroscopy for Chemical Analysis (ESCA) before and after reduction in 40 Torr of CO for 1 hour at various temperatures from 75 to 175 C. The reduction results in loss of surface oxygen, formation of metallic tin, conversion of platinum oxides to Pt-O-Sn and Pt(OH)2 and a small amount of metallic Pt which alloys with the tin. These results should be useful in understanding how the pretreatment temperature affects the catalytic activity of platinized tin oxide toward CO oxidation.

Drawdy, Jean E.↗

An Investigation of the Electrical Short Circuit Characteristics of Tin Whiskers

Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that has a currently unknown probability associated with it. Due to contact resistance electrical shorts may not occur at lower voltage levels. In this experiment, we study the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From this data we can estimate the probability of an electrical short, as a function of voltage, given that a free tin whisker has bridged two adjacent exposed electrical conductors. Also, three tin whiskers grown from the same Space Shuttle Orbiter card guide used in the aforementioned experiment were cross-sectioned and studied using a focused ion beam (FIB). The rare polycrystalline structure seen in the FIB cross section was confirmed using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size to determine that the tin plating on the card guides had a bright finish.

Courey, Karim J.↗

An Investigation of the Electrical Short Circuit Characteristics of Tin Whiskers

In this experiment, an empirical model to quantify the probability of occurrence of an electrical short circuit from tin whiskers as a function of voltage was developed. This model can be used to improve existing risk simulation models FIB and TEM images of a tin whisker confirm the rare polycrystalline structure on one of the three whiskers studied. FIB cross-section of the card guides verified that the tin finish was bright tin.

Courey, Karim J.↗

An Investigation of the Electrical Short Circuit Characteristics of Tin Whiskers

Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that has a currently unknown probability associated with it. Due to contact resistance electrical shorts may not occur at lower voltage levels. In this experiment, we study the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From this data we can estimate the probability of an electrical short, as a function of voltage, given that a free tin whisker has bridged two adjacent exposed electrical conductors. Also, three tin whiskers grown from the same Space Shuttle Orbiter card guide used in the aforementioned experiment were cross-sectioned and studied using a focused ion beam (FIB). The rare polycrystalline structure seen in the FIB cross section was confirmed using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size to determine that the tin plating on the card guides had a bright finish.

Courey, Karim J.↗

An Empirical Model for Estimating the Probability of Electrical Short Circuits from Tin Whiskers

In this experiment, an empirical model to quantify the probability of occurrence of an electrical short circuit from tin whiskers as a function of voltage was developed. This empirical model can be used to improve existing risk simulation models. FIB and TEM images of a tin whisker confirm the rare polycrystalline structure on one of the three whiskers studied. FIB cross-section of the card guides verified that the tin finish was bright tin.

Courey, Karim↗

Optimization of Aluminum-Tin Ink Composition and Sintering in Atmospheric Conditions

This study will focus on the basics of generating an aluminum-tin ink that can sinter in air and exhibits properties near that of a solid aluminum-tin alloy. Sintering temperatures will also be assessed in this study. Once the optimal aluminum ink composition is determined, the optimal ink thickness for homogeneous sintering must be determined by additional experimentation. Additive manufacturing is a rapidly developing and growing manufacturing process and has proven successful in many different ways. Processes, such as extrusion three-dimensional (3D) printing and selective laser melting (SLM), have proven to work but have limitations, such as material capabilities or density issues. SLM is a revolutionary process for additive manufacturing of metals but cannot be used in outer space due to the need for metallic powder which would diffuse into the atmosphere in a zero-gravity environment. For this reason, metallic ink additive manufacturing is a potential solution. Work is being done on metallic ink additive manufacturing in a vacuum for electrical applications. This project has focused on developing an aluminum-tin metallic ink that can sinter without the need of a vacuum or inert gas-purged atmosphere in order to prevent oxidation of the aluminum by adding flux. Once a potential ink composition has been determined through sintering of small disks and thin layers of ink, the ink may be studied with a multimaterial 3D printer at NASA Marshall Space Flight Center (MSFC) in future experiments. If successful, this aluminum-tin ink will be capable for use on the International Space Station to make replacement parts quickly. Along with its zero-gravity advantages, this ink may also have applications on Earth because it may be extruded on a substrate with precise ceramic tips in a 3D printing process. This would allow the fabrication of precise, complex shapes and may generate a much faster and more efficient printing process as compared with traditional powder bed additive manufacturing processes. The process would not be limited by a small building volume because the system would not require an enclosed chamber.

Courtright, Z. S.↗

Methods for chemical recovery of non-carrier-added radioactive tin from irradiated intermetallic Ti-Sb targets

The invention provides a method of chemical recovery of no-carrier-added radioactive tin (NCA radiotin) from intermetallide TiSb irradiated with accelerated charged particles. An irradiated sample of TiSb can be dissolved in acidic solutions. Antimony can be removed from the solution by extraction with dibutyl ether. Titanium in the form of peroxide can be separated from tin using chromatography on strong anion-exchange resin. In another embodiment NCA radiotin can be separated from iodide solution containing titanium by extraction with benzene, toluene or chloroform. NCA radiotin can be finally purified from the remaining antimony and other impurities using chromatography on silica gel. NCA tin-117m can be obtained from this process. NCA tin-117m can be used for labeling organic compounds and biological objects to be applied in medicine for imaging and therapy of various diseases.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Method of manufacturing tin-doped indium oxide nanofibers

A method of making indium tin oxide nanofibers includes the step of mixing indium and tin precursor compounds with a binder polymer to form a nanofiber precursor composition. The nanofiber precursor composition is co-formed with a supporting polymer to form a composite nanofiber having a precursor composition nanofiber completely surrounded by the supporting polymer composition. The supporting polymer composition is removed from the composite nanofiber to expose the precursor composition nanofiber. The precursor composition nanofiber is then heated in the presence of oxygen such as O.sub.2 to form indium tin oxide and to remove the binder polymer to form an indium tin oxide nanofiber. A method of making metal oxide nanofibers is also disclosed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Corrosion Testing of TiN on Steel Substrates for use in Waste Packages

An outer shield barrier for spent nuclear fuel casks is being developed in order to improve dry cask performance under mechanical, chemical, and radiological burdens. The materials proposed for the outer shield barrier are titanium nitride (TiN), a composite oxide layer consisting of ZrO{sub 2}, TiO{sub 2}, and Al{sub 2}O{sub 3}, and a final layer of molybdenum disulfide (MoS{sub 2}). A proposed multilayer and multicomposite approach are being investigated in order to optimize the outer shield barriers performance. Spent nuclear fuel casks are frequently made, in part, of 304 and 316 stainless steels. These materials have been chosen as substrates to deposit single layer films of the proposed materials. In order to understand how these materials will behave layered and composited it is first necessary to understand how they perform individually. Several corrosion studies have been performed and analyzed for cyclic corrosion and static corrosion in different brine solutions and at different temperatures. The corrosion rate, over potential, activation enthalpy, and entropy of corrosion have been documented in previous publications. One of the main functions of the TiN coating is to serve as a corrosion barrier on the waste package. In this study we investigate pitting corrosion on thin layers of TiN through cyclic polarization testing and scanning electron microscopy. The corrosion protection of thin layers of TiN has been investigated on 304 and 316 stainless steels. Cyclic polarization testing has been used to this end. Corrosion rates have been calculated using tefel fits on data obtained from this testing and SEM images were used in conjunction with this data. Pitting is observed to occur even at the thickest deposition conditions tested. Although the corrosion rates decrease at these thicker values - sometimes dramatically - thicker layers will be deposited in the future to provide complete resistance to pitting. Deposition and testing of these layers is currently underway. (authors)

36 MATERIALS SCIENCE↗

Alkaline earth metal doped tin oxide as a novel oxygen storage material

Alkaline earth metal doped tin oxide (SnO{sub 2}) hollow nanospheres with a diameter of 50 nm have been synthesized successfully via a facial solvothermal route in a very simple system composed of only ethanol, acetic acid, SnCl{sub 4}·5H{sub 2}O and A(NO{sub 3}){sub 2}·xH{sub 2}O (A = Mg, Ca, Sr, Ba). The synthesized undoped SnO{sub 2} and A-doped SnO{sub 2} hollow nanospheres were characterized by the oxygen storage capacity (OSC), X-ray diffraction, transmission electron microscopy and the Brunauer–Emmet–Teller (BET) technique. The OSC values of all samples were measured using thermogravimetric-differential thermal analysis. The incorporation of alkaline earth metal ion into tin oxide greatly enhanced the thermal stability and OSC. Especially, Ba-doped SnO{sub 2} hollow nanospheres calcined at 1000 °C for 20 h with a BET surface area of 61 m{sup 2} g{sup −1} exhibited the considerably high OSC of 457 μmol-O g{sup −1} and good thermal stability. Alkaline earth metal doped tin oxide has the potential to be a novel oxygen storage material.

36 MATERIALS SCIENCE↗

Electron exchange between tin impurity U{sup –} centers in PbS{sub z}Se{sub 1–z} alloys

Using emission {sup 119mm}Sn({sup 119m}Sn) and {sup 119}Sb({sup 119m}Sn) Mössbauer spectroscopy, it is shown that impurity tin atoms in PbS{sub z}Se{sub 1–z} alloys substitute lead atoms and are two-electron donors with negative correlation energy (U{sup –} centers). It is found that the energy levels related to impurity tin atoms are in the lower half of the band gap at z ≥ 0.5 against the background of allowed valence-band states at z ≤ 0.4. The electron exchange between neutral and doubly ionized tin U{sup –} centers in partially compensated Pb{sub 0.99}Sn{sub 0.005}Na{sub 0.005}S{sub z}Se{sub 1–z} alloys is studied. The activation energy of this process decreases from 0.111(5) eV for a composition with z = 1 to 0.049(5) eV for compositions with c ≤ 0. For all z, the exchange is implemented via the simultaneous transfer of two electrons using delocalized valence-band states.

36 MATERIALS SCIENCE↗

Influence of current density on microstructure of pulse electrodeposited tin coatings

Pulse electrodeposited tin coatings on copper substrate have been synthesized from an aqueous solution containing sodium stannate (Na{sub 2}SnO{sub 3}.3H{sub 2}O) and sodium hydroxide (NaOH). The effect of current density on surface morphology of the deposits has been investigated. As deposited coatings are characterized by X-ray diffraction, scanning electron microscopy, electron backscatter diffraction, and line profile analysis. The X-ray diffraction analysis shows that the deposits consist of tetragonal ({beta}-Sn) structure with microcrystalline grains. The deposits plated at lower current density exhibit (110) texture which decreases with increasing current densities. The effects of current density on Cu-Sn diffusion and whisker growth of the electrodeposited tin coatings are also reported here. - Highlights: Black-Right-Pointing-Pointer Pulse electrodeposition of Sn from aqueous alkaline solution without adding any organic additive. Black-Right-Pointing-Pointer Effect of current density on morphology and whisker growth in tin coatings aged for 1 year. Black-Right-Pointing-Pointer Solution bath is stable and can be operated over a wide range of current density.

36 MATERIALS SCIENCE↗

Evolution of microstructure and grain boundary character distribution of a tin bronze annealed at different temperatures

Specimens cut from a rolled tin bronze sheet were annealed at 400–800 °C for 1 h and evolution of their microstructures was then characterized in details by electron channeling contrast imaging and electron backscatter diffraction techniques. Particularly, statistics on special boundaries (SBs) with Σ ≤ 29 and network connectivity of random high angle boundaries (HABs) in the annealed specimens were examined to probe optimization potentials of grain boundary character distribution (GBCD) for this material. Results show that the deformed microstructure in the as-received material begins to be recrystallized when the annealing temperature increase to 500 °C and average grain sizes surge with further increasing temperatures. As a result of the recrystallization, a large number of annealing twins (with Σ3 misorientation) are produced, leading to remarkably increased fractions of SBs (f{sub SBs}). Thanks to preexisting dense low angle boundaries, the majority of SBs in the 500 °C specimen with only partial recrystallization are Σ3{sub ic} (incoherent) boundaries, which effectively disrupt connectivity of random HABs network. Although the f{sub SBs} can be further increased (up to 72.5%) in specimens with full recrystallization (at higher temperatures), the Σ3{sub ic} boundaries would be replaced to some extent by Σ3{sub c} (coherent) boundaries which do not contribute directly to optimizing the GBCD. This work should be able to provide clear suggestions on applying the concept of grain boundary engineering to tin bronze alloys. - Highlights: • The rolled tin bronze begins to be recrystallized as temperature increases to 500 °C. • A lot of SBs are produced after recrystallization and the highest f{sub SBs} is 72.5%. • Partially recrystallized specimen has the optimum GBCD due to more Σ3{sub ic} boundaries. • The Σ3{sub ic} boundaries are replaced by Σ3{sub c} boundaries after full recrystallization.

36 MATERIALS SCIENCE↗