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At least 559 records · Page 31
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Fabrication of Engineered Silica-Functionalized-Polyanilines Nanocomposites for Water Decontamination of Cadmium and Lead

In this study, two novel functionalized silica nanocomposites were synthesized via covalent bonding with nanopolyaniline (NPANI) and crosslinked nanopolyaniline (CrossNPANI) to produce [NSi-NPANI] and [NSi-CrossNPANI], respectively. The two nanocomposites were portrayed by SEM, FT-IR, HR-TEM, BET-surface and TGA. The HR-TEM images of [NSi-NPANI] and [NSi-CrossNPANI] confirmed the particle size in the range 14.28–21.43 and 26.19–35.71 nm, respectively and these two nanocomposites were successfully applied to remove divalent cadmium and lead from solutions. As compared to nanosilica [NSi] sorbent, the maximum capacity values of the two nanocomposites for divalent cadmium and lead were identified to increase from 100–250 µmole g{sup −1} (pH 1.0) to 750–800 µmole g{sup −1} (pH 7.0) and from 400–1050 µmole g{sup −1} (pH 1.0) to 650–1350 µmole g{sup −1} (pH 6.0), at the optimum conditions. The adsorption data were compared using two and three parameter equations based on Langmuir, Freundlich, Temkin, Dubinin-Radushkevich, Redlish-Peterson and sips models. The kinetic study of [NSi-NPANI] and [NSi-CrossNPANI] revealed that the pseudo-second order kinetic was the best model to explain the kinetic data for cadmium(II) and lead(II). The free energy of sorption (ΔG{sup o}), enthalpy (ΔH{sup o}), and entropy (ΔS{sup o}) changes were calculated to portend the nature of adsorption. Adsorptive extraction of toxic lead and cadmium from tap water and wastewater was successfully accomplished with the range of percentage recovery values 98.5–100.0 and 91.9–93.0%, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2012

Inverse association of intellectual function with very low blood lead but not with manganese exposure in Italian adolescents

Background: Pediatric lead (Pb) exposure impacts cognitive function and behavior and co-exposure to manganese (Mn) may enhance neurotoxicity. Objectives: To assess cognitive and behavioral function in adolescents with environmental exposure to Pb and Mn. Methods: In this cross sectional study, cognitive function and behavior were examined in healthy adolescents with environmental exposure to metals. The Wechsler Intelligence Scale for Children (WISC) and the Conners-Wells' Adolescent Self-Report Scale Long Form (CASS:L) were used to assess cognitive and behavioral function, respectively. ALAD polymorphisms rs1800435 and rs1139488 were measured as potential modifiers. Results: We examined 299 adolescents (49.2% females) aged 11-14 years. Blood lead (BPb) averaged 1.71 {mu}g/dL (median 1.5, range 0.44-10.2), mean Blood Manganese (BMn) was 11.1 {mu}g/dL (median 10.9, range 4.00-24.1). Average total IQ was 106.3 (verbal IQ=102, performance IQ=109.3). According to a multiple regression model considering the effect of other covariates, a reduction of about 2.4 IQ points resulted from a two-fold increase of BPb. The Benchmark Level of BPb associated with a loss of 1 IQ-point (BML01) was 0.19 {mu}g/dL, with a lower 95% confidence limit (BMLL01) of 0.11 {mu}g/dL. A very weak correlation resulted between BPb and the ADHD-like behavior (Kendall's tau rank correlation=0.074, p=0.07). No influence of ALAD genotype was observed on any outcome. Manganese was not associated with cognitive and behavioral outcomes, nor was there any interaction with lead. Conclusions: These findings demonstrate that very low level of lead exposure has a significant negative impact on cognitive function in adolescent children. Being an essential micro-nutrient, manganese may not cause cognitive effects at these low exposure levels.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Metal residues, histopathology and presence of parasites in the liver and gills of fourhorn sculpin (Myoxocephalus quadricornis) and shorthorn sculpin (Myoxocephalus scorpius) near a former lead-zinc mine in East Greenland

Fourhorn sculpins (Myoxocephalus quadricornis) and shorthorn sculpins (Myoxocephalus scorpius) have been considered suitable local bioindicators for environmental monitoring studies in the Arctic. Because these species share many characteristics, data from the two species have previously been pooled when assessing marine metal contamination. A chemical and histological study was conducted on fourhorn and shorthorn sculpins collected around a contaminated lead-zinc mine at East Greenland to investigate whether there were any differences in the residues of metals, histopathology and parasites in liver and gills between the two sculpin species. The results demonstrated that concentrations of copper (Cu), zinc (Zn), mercury (Hg) and lead (Pb) were significantly higher in the fourhorn sculpins (p<0.001) while there were no significant differences for arsenic (As) or cadmium (Cd). Furthermore, density of blood vessel fibrosis (p=0.028), prevalence and density of chondroplasia (p=0.002 and p=0.005, respectively), number of mucin-containing mucous cells (p<0.001) and chloride cells (p<0.001) and mean intensity of colonial Peritricha (p<0.001) were significantly higher in fourhorn sculpin. Based on these results we suggest that pooling the two species when conducting environmental assessments is not recommended as it can lead to incorrect conclusions. We propose that a larger study investigating the biological effects of zinc-lead mining in Greenland is needed. - Highlights: • Fourhorn sculpins (Myoxocephalus quadricornis) more sensitive to pollution than shorthorn sculpins (Myoxocephalus scorpius). • Metal residues, histological changes and presence of parasites were species-specific. • Different sculpin species should not be pooled together as pollution biomarkers.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2011

Lead sheathing of ship hulls in the Roman period: Archaeometallurgical characterisation

An archaeometallurgical analysis of samples of lead sheathing from five ships of the Roman period was carried out in order to determine their composition and microstructure, and to obtain a better understanding of their manufacturing processes. The examinations included optical microscopy of metallographic cross-sections, microhardness tests, scanning electron microscopy, including energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. The results show that the samples were all composed of lead covered with an oxide layer. The sheet thicknesses, microhardness values and microhardness distribution, as well as the grain size distribution, led to the conclusion that all of the sheets were produced by the same technology, using hammering, and were probably used for the same purpose. The presence of antimony was observed in the sample from the Roman ship from Caesarea, which may hint at an Italian (Sardinian) origin of the material, and perhaps of the ship. - Research Highlights: {yields} During the Roman period ship hulls were sheathed with lead. {yields} Five samples have been analysed for their characteristics and manufacturing process. {yields} The process was cold-working (strain-hardening) using hammering. {yields} The lead was open-casted on a flat stone, and later hammered at room temperature. {yields} Antimony in the Caesarea shipwreck may indicate an Italian origin of construction.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effects of metallic nanoparticle doped flux on the interfacial intermetallic compounds between lead-free solder ball and copper substrate

Lead free solders currently in use are prone to develop thick interfacial intermetallic compound layers with rough morphology which are detrimental to the long term solder joint reliability. A novel method has been developed to control the morphology and growth of intermetallic compound layers between lead-free Sn–3.0Ag–0.5Cu solder ball and copper substrate by doping a water soluble flux with metallic nanoparticles. Four types of metallic nanoparticles (nickel, cobalt, molybdenum and titanium) were used to investigate their effects on the wetting behavior and interfacial microstructural evaluations after reflow. Nanoparticles were dispersed manually with a water soluble flux and the resulting nanoparticle doped flux was placed on copper substrate. Lead-free Sn–3.0Ag–0.5Cu solder balls of diameter 0.45 mm were placed on top of the flux and were reflowed at a peak temperature of 240 °C for 45 s. Angle of contact, wetting area and interfacial microstructure were studied by optical microscopy, field emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. It was observed that the angle of contact increased and wetting area decreased with the addition of cobalt, molybdenum and titanium nanoparticles to flux. On the other hand, wettability improved with the addition of nickel nanoparticles. Cross-sectional micrographs revealed that both nickel and cobalt nanoparticle doping transformed the morphology of Cu{sub 6}Sn{sub 5} from a typical scallop type to a planer one and reduced the intermetallic compound thickness under optimum condition. These effects were suggested to be related to in-situ interfacial alloying at the interface during reflow. The minimum amount of nanoparticles required to produce the planer morphology was found to be 0.1 wt.% for both nickel and cobalt. Molybdenum and titanium nanoparticles neither appear to undergo alloying during reflow nor have any influence at the solder/substrate interfacial reaction. Thus, doping of flux with appropriate metallic nanoparticles can be successfully used to control the morphology and growth of intermetallic compound layers at the solder/substrate interface which is expected to lead to better reliability of electronic devices. - Highlights: • A novel nanodoped flux method has been developed to control the growth of IMCs. • Ni doped flux improves the wettability, but Co, Mo and Ti deteriorate it. • Ni and Co doped flux gives planer IMC morphology through in-situ alloying effect. • 0.1 wt.% Ni and Co addition into flux gives the lowest interfacial IMC thickness. • Mo and Ti doped flux does not have any influence at the interfacial reaction.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Improvement of Varian a-Si EPID dosimetry measurements using a lead-shielded support-arm

Dosimetry measurements with Varian amorphous silicon electronic portal imaging devices (a-Si EPIDs) are affected by the backscattered radiation from the EPID support arm. In this study, the nonuniform backscatter from an E-type support arm was reduced by fixing a thick (12.2 Multiplication-Sign 10.5 Multiplication-Sign 0.5 cm{sup 3}) piece of lead on top of the arm, and the remaining backscatter was modeled and included in an existing dose prediction algorithm. The applied backscatter kernel was the average of kernels on different regions of the EPID over the arm. The lead-shielded arm reduced the nonuniform backscatter component by about 50% for field sizes ranging from 3 Multiplication-Sign 3 to 30 Multiplication-Sign 30 cm{sup 2} and the field symmetry improved for medium to large fields up to 3%. Gamma evaluation of the measured and modeled doses (2%, 2-mm criteria) showed that using the lead-shielded arm in the model increased the number of points with Gamma index <1 by 5.7% and decreased the mean Gamma by 0.201. Even using the lead alone (no modeling) could increase the number of points with Gamma index <1 by 4.7% and decrease the mean Gamma by 0.153. This is a simple and easy method to decrease the nonuniform arm backscatter and improve the accuracy of dosimetry measurements with the existing EPIDs used for clinical applications.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2019

Toward Stable Deep-Blue Luminescent Colloidal Lead Halide Perovskite Nanoplatelets: Systematic Photostability Investigation

Colloidal lead halide perovskite nanocrystals and nanoplatelets have emerged as promising semiconductor nanomaterials because of their spectral tunability, facile processability, and bright emission with high color purity. In particular, strong quantum and dielectric confinement make atomically thin colloidal lead bromide perovskite nanoplatelets a favorable candidate for next-generation deep-blue-emitting (λ max = 437 nm) materials. However, poor photostability poses a critical challenge; colloidal nanoplatelets suffer from photobleaching or transformation into thicker, less-confined nanostructures with red-shifted emission upon UV irradiation. In this study, we synthesize deep-blue-emitting organic–inorganic hybrid perovskite nanoplatelets (formula: L 2 [ABX 3 ]BX 4 , L: butylammonium and octylammonium, A: methylammonium or formamidinium, B: lead, and X: bromide or iodide) with large lateral dimension (~1 μm) by ligand-assisted reprecipitation and systematically investigate the factors that affect the photostability of those nanoplatelets. We find that freshness of the prepared precursor solutions for ligand-assisted reprecipitation is critical to obtain better stability with high photoluminescence quantum yield of perovskite nanoplatelets. Photobleaching is found to result from intrinsic instability of the perovskite lattice against UV irradiation in nanoplatelets, whereas transformation into thicker nanostructures results from extrinsic factors—moisture, primarily. Furthermore, we observe that substitution of the organic cation from formamidinium to methylammonium and addition of excess alkylammonium bromide ligands significantly enhance both the ambient and photostability. Lastly, we demonstrate that the dropcast film of methylammonium lead bromide nanoplatelets with excess alkylammonium bromide ligands shows dramatically improved stability both under UV irradiation and under ambient conditions. Lastly, this study expands our understanding of the factors that affect perovskite nanoplatelet photostability and opens up new possibilities for the fabrication of stable perovskite nanoplatelet-based optoelectronic devices.

2D↗
DOE OSTI2020

Lead-free Cesium Europium Halide Perovskite Nanocrystals

Because of the toxicity of lead, searching for a lead-free halide perovskite semiconducting material with comparable optical and electronic properties is of great interest. Rare-earth-based halide perovskite represents a promising class of materials for this purpose. In this work, we demonstrate the solution-phase synthesis of single-crystalline CsEuCl 3 nanocrystals with a uniform size distribution centered around 15 nm. The CsEuCl 3 nanocrystals have photoluminescence emission centered at 435 nm, with a full width at half-maximum of 19 nm. Furthermore, CsEuCl 3 nanocrystals can be embedded in a polymer matrix that provides enhanced stability under continuous laser irradiation. Lead-free rare-earth cesium europium halide perovskite nanocrystals represent a promising candidate to replace lead halide perovskites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

The Making and Breaking of Lead-Free Double Perovskite Nanocrystals of Cesium Silver–Bismuth Halide Compositions

Replacing lead in halide perovskites is of great interest due to concerns about stability and toxicity. Recently, lead free double perovskites in which the unit cell is doubled and two divalent lead cations are substituted by a combination of mono- and trivalent cations have been synthesized as bulk single crystals and as thin films. In this report, we investigate stability and optical properties of all-inorganic cesium silver(I) bismuth(III) chloride and bromide nanocrystals with the double perovskite crystal structure. The cube-shaped nanocrystals are monodisperse in size with typical side lengths of 8 to 15 nm. The absorption spectrum of the nanocrystals presents a sharp peak, which we assign to a direct bismuth s-p transition and not to a quantum confined excitonic transition. Using this spectroscopic handle combined with high-resolution transmission electron microscopy (TEM) based elemental analysis, we conduct stoichiometric studies at the single nanocrystal level as well as decomposition assays in solution and observe that Ag+ diffusion and coalescence is one of the pathways by which this material degrades. Drying the nanocrystals leads to self-assembly into ordered nanocrystal solids, and these exhibit less degradation than nanocrystals in solution. Our results show that Cs 2 AgBiX 6 (X = Cl, Br) nanocrystals are a useful model system to study structure-function relationships in the search for stable nontoxic halide perovskites.

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

Synergistic effects of lead thiocyanate additive and solvent annealing on the performance of wide-bandgap perovskite solar cells

Here, we show that the cooperation of lead thiocyanate additive and a solvent annealing process can effectively increase the grain size of mixed-cation lead mixed-halide perovskite thin films while avoiding excess lead iodide formation. As a result, the average grain size of the wide-bandgap mixed-cation lead perovskite thin films increases from 66 ± 24 to 1036 ± 111 nm, and the mean carrier lifetime shows a more than 3-fold increase, from 330 ns to over 1000 ns. Consequently, the average open-circuit voltage of wide-bandgap perovskite solar cells increases by 80 (70) mV, and the average power conversion efficiency (PCE) increases from 13.44 ± 0.48 (11.75 ± 0.34) to 17.68 ± 0.36 (15.58 ± 0.55)% when measured under reverse (forward) voltage scans. The best-performing wide-bandgap perovskite solar cell, with a bandgap of 1.75 eV, achieves a stabilized PCE of 17.18%.

14 SOLAR ENERGY↗
DOE OSTI2014

Efficient methylammonium lead iodide perovskite solar cells with active layers from 300 to 900 nm

Efficient methylammonium lead iodide perovskite-based solar cells have been prepared in which the perovskite layer is sandwiched in between two organic charge transporting layers that block holes and electrons, respectively. This configuration leads to stable and reproducible devices that do not suffer from strong hysteresis effects and when optimized lead to efficiencies close to 15%. The perovskite layer is formed by using a dual-source thermal evaporation method, whereas the organic layers are processed from solution. The dual-source thermal evaporation method leads to smooth films and allows for high precision thickness variations. Devices were prepared with perovskite layer thicknesses ranging from 160 to 900 nm. The short-circuit current observed for these devices increased with increasing perovskite layer thickness. The main parameter that decreases with increasing perovskite layer thickness is the fill factor and as a result optimum device performance is obtained for perovskite layer thickness around 300 nm. However, here we demonstrate that with a slightly oxidized electron blocking layer the fill factor for the solar cells with a perovskite layer thickness of 900 nm increases to the same values as for the devices with thin perovskite layers. As a result the power conversion efficiencies for the cells with 300 and 900 nm are very similar, 12.7% and 12%, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Phase transformation and growth mechanism of RF sputtered ferroelectric lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 ) films

Lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 , PST), an order/disorder ferroelectric, is a potential candidate for electrocaloric cooling and pyroelectric infrared (IR) detector. In this work, we report the phase transformation kinetics from two series of samples containing pure amorphous and mixture of amorphous and pyrochlore to desired perovskite phase using postdeposition rapid thermal processing (RTP) as well as growth mechanism of RF sputtered PST thin films using excess lead target on platinized silicon (Pt/Ti/SiO 2 /Si) substrates. We find that small changes in the temperature ramp have a large effect on the degree of perovskite conversion (ferroelectric phase), orientation (crystallographic texture), and long-range order parameter (< S 111 >). Through isothermal annealing, we obtained optimal perovskite phase at ≥700°C temperature. The phase transformation is characterized by spontaneous formation of center-type in-plane radial rosette-like structures revealed by scanning electron microscopy. The PST perovskite crystallites were found to coexist with pyrochlore in RTP annealed films. The volume fractions for perovskite and pyrochlore phase were obtained from the analysis of “rosettes” and respective X-ray diffraction intensities which helped to determine various parameters associated with phase kinetics (n, k, and activation energy, Ea) and accompanying growth. The effective activation energies of perovskite transition and growth were found to be 332 ± 11 kJ/mol (345 ± 11 kJ/mol) and 114 ± 10 kJ/mol (122 ± 10 kJ/mol), respectively, for pure amorphous only (and mixed amorphous and pyrochlore) phase following nucleation-growth controlled Avrami's equation. A linear growth rate (n~1) for the perovskite phase indicates predominant interface-controlled process and diffusion-limited phenomena thus inhibiting rosette size owing to reactant depletion and soft impingement at the grain boundary. However, the growth behavior is isotropic in two-dimension parallel to the plane of the substrates for both sample series. Furthermore, lead loss was severe for in-situ growth and RTP combined with conventional furnace annealing than those of RTP only films, which were closer to stoichiometric albeit with excess lead and marginal oxygen vacancies (V o ).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Size Dependences of the Magnetic Properties of Superconducting Lead–Porous Glass Nanostructures

Superconducting structures Pb–PG formed by filling a porous glass matrix with the lead from melt under pressure have been investigated. Samples with characteristic pore structure diameters of d ≈ 7, 3, and 2 nm have been studied. It has been found that the critical temperature of the superconducting transition in the samples under study is similar to the corresponding value T{sub c} ≈ 7.2 K for bulk lead. At the same time, it has been observed that the critical magnetic field of the nanocomposites, which attains H{sub c}(T = 0 K) ≈ 165 kOe for Pb–PG (3 nm), exceeds several times the value H{sub c}(0) = 803 Oe for bulk lead. The low-temperature magnetic- field dependences of magnetic moment M(H) contain quasi-periodic flux jumps, which vanish with a decrease in the lead nanostructure diameter. A qualitative model of the observed effects is considered.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

CASTELO: clustered atom subtypes aided lead optimization—a combined machine learning and molecular modeling method

Background: Drug discovery is a multi-stage process that comprises two costly major steps: pre-clinical research and clinical trials. Among its stages, lead optimization easily consumes more than half of the pre-clinical budget. We propose a combined machine learning and molecular modeling approach that partially automates lead optimization workflow in silico, providing suggestions for modification hot spots. Results: The initial data collection is achieved with physics-based molecular dynamics simulation. Contact matrices are calculated as the preliminary features extracted from the simulations. To take advantage of the temporal information from the simulations, we enhanced contact matrices data with temporal dynamism representation, which are then modeled with unsupervised convolutional variational autoencoder (CVAE). Finally, conventional and CVAE-based clustering methods are compared with metrics to rank the submolecular structures and propose potential candidates for lead optimization. Conclusion: With no need for extensive structure-activity data, our method provides new hints for drug modification hotspots which can be used to improve drug potency and reduce the lead optimization time. It can potentially become a valuable tool for medicinal chemists.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2011

Understanding the function and performance of carbon-enhanced lead-acid batteries : milestone report for the DOE Energy Storage Systems Program (FY11 Quarter 4: July through September 2011).

This report describes the status of research being performed under CRADA No. SC10/01771.00 (Lead/Carbon Functionality in VRLA Batteries) between Sandia National Laboratories and East Penn Manufacturing, conducted for the U.S. Department of Energy's Energy Storage Systems Program. The Quarter 4 Milestone was completed on time. The milestone entails the initiation of high rate, partial state of charge (HRPSoC) cycling of the carbon enhanced batteries. The morphology, porosity, and porosity distribution within the plates after 1k and 10k cycles were documented, illustrating the changes which take place in the early life of the carbon containing batteries, and as the battery approaches failure due to hard sulfation for the control battery. Longer term cycling on a subset of the received East Penn cells containing different carbons (and a control) continues, and will progress into FY12. Carbon has been explored as an addition to lead-acid battery electrodes in a number of ways. Perhaps the most notable to date has been the hybrid 'Ultrabattery' developed by CSIRO where an asymmetric carbon-based electrochemical capacitor is combined with a lead-acid battery into a single cell, dramatically improving high-rate partial-state-of-charge (HRPSoC) operation. As illustrated below, the 'Ultrabattery' is a hybrid device constructed using a traditional lead-acid battery positive plate (i.e., PbO2) and a negative electrode consisting of a carbon electrode in parallel with a lead-acid negative plate. This device exhibits a dramatically improved cycle life over traditional VRLA batteries, as well as increased charge power and charge acceptance. The 'Ultrabattery' has been produced successfully by both The Furukawa Battery Co. and East Penn Manufacturing. An example illustrating the dramatic improvement in cycle life of the Ultrabattery over a conventional VRLA battery is shown in a graph. In addition to the aforementioned hybrid device, carbon has also been added directly to traditional VRLA batteries as an admixture in both the positive and negative plates, the latter of which has been found to result in similar improvements to battery performance under high-rate partial-state-of-charge (HRPSoC) operation. It is this latter construction, where carbon is added directly to the negative active material (NAM) that is the specific incarnation being evaluated through this program. Thus, the carbon-modified (or Pb-C) battery (termed the 'Advanced' VRLA battery by East Penn Manufacturing) is a traditional VRLA battery where an additional component has been added to the negative electrode during production of the negative plate. The addition of select carbon materials to the NAM of VRLA batteries has been demonstrated to increase cycle life by an order of magnitude or more under (HRPSoC) operation. Additionally, battery capacity increases on cycling and, in fact, exceeds the performance of the batteries when new.

25 ENERGY STORAGE↗
DOE OSTI2017

Low Pressure Vapor-assisted Solution Process for Tunable Band Gap Pinhole-free Methylammonium Lead Halide Perovskite Films

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, we present a protocol for the fabrication of this material via the low-pressure vapor assisted solution process (LP-VASP) method, which yields ~19% power conversion efficiency in planar heterojunction perovskite solar cells. First, we report the synthesis of methylammonium iodide (CH 3 NH 3 I) and methylammonium bromide (CH 3 NH 3 Br) from methylamine and the corresponding halide acid (HI or HBr). Then, we describe the fabrication of pinhole-free, continuous methylammonium-lead halide perovskite (CH 3 NH 3 PbX 3 with X = I, Br, Cl and their mixture) films with the LP-VASP. This process is based on two steps: i) spin-coating of a homogenous layer of lead halide precursor onto a substrate, and ii) conversion of this layer to CH 3 NH 3 PbI 3-x Br x by exposing the substrate to vapors of a mixture of CH 3 NH 3 I and CH 3 NH 3 Br at reduced pressure and 120 °C. Through slow diffusion of the methylammonium halide vapor into the lead halide precursor, we achieve slow and controlled growth of a continuous, pinhole-free perovskite film. The LP-VASP allows synthetic access to the full halide composition space in CH 3 NH 3 PbI 3-x Br x with 0 ≤ x ≤ 3. Depending on the composition of the vapor phase, the bandgap can be tuned between 1.6 eV ≤ E g ≤ 2.3 eV. In addition, by varying the composition of the halide precursor and of the vapor phase, we can also obtain CH 3 NH 3 PbI 3-x Cl x . Films obtained from the LP-VASP are reproducible, phase pure as confirmed by X-ray diffraction measurements, and show high photoluminescence quantum yield. The process does not require the use of a glovebox.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2014

NASA-DoD Lower Process Temperature Lead-Free Solder Project Overview

This project is a follow-on effort to the Joint Council on Aging AircraftJoint Group on Pollution Prevention (JCAAJG-PP) Pb-free Solder Project and NASA-DoD Lead-Free Electronics Project which were the first projects to test the reliability of Pb-free solder joints against the requirements of the aerospace and military community. This effort would continue to build on the results from the JCAAJG-PP Lead-Free Solder Project and NASA-DoD Lead-Free Electronics Project while focusing on a particular failure mechanism currently plaguing Pb-free assemblies, pad cratering.The NASA-DoD Lead-Free Electronics Project confirmed that pad cratering is one of the dominant failure modes that occur in various board level reliability tests, especially under dynamic loading. Pad Cratering is a latent defect that may occur during assembly, rework, and post assembly handling and testing.

electronics↗
DOE OSTI2015

Effects of sulfur on lead partitioning during sludge incineration based on experiments and thermodynamic calculations

Highlights: • A thermodynamic equilibrium calculation was carried out. • Effects of three types of sulfurs on Pb distribution were investigated. • The mechanism for three types of sulfurs acting on Pb partitioning were proposed. • Lead partitioning and species in bottom ash and fly ash were identified. - Abstract: Experiments in a tubular furnace reactor and thermodynamic equilibrium calculations were conducted to investigate the impact of sulfur compounds on the migration of lead (Pb) during sludge incineration. Representative samples of typical sludge with and without the addition of sulfur compounds were combusted at 850 °C, and the partitioning of Pb in the solid phase (bottom ash) and gas phase (fly ash and flue gas) was quantified. The results indicate that three types of sulfur compounds (S, Na{sub 2}S and Na{sub 2}SO{sub 4}) added to the sludge could facilitate the volatilization of Pb in the gas phase (fly ash and flue gas) into metal sulfates displacing its sulfides and some of its oxides. The effect of promoting Pb volatilization by adding Na{sub 2}SO{sub 4} and Na{sub 2}S was superior to that of the addition of S. In bottom ash, different metallic sulfides were found in the forms of lead sulfide, aluminosilicate minerals, and polymetallic-sulfides, which were minimally volatilized. The chemical equilibrium calculations indicated that sulfur stabilizes Pb in the form of PbSO{sub 4}(s) at low temperatures (<1000 K). The equilibrium calculation prediction also suggested that SiO{sub 2}, CaO, TiO{sub 2}, and Al{sub 2}O{sub 3} containing materials function as condensed phase solids in the temperature range of 800–1100 K as sorbents to stabilize Pb. However, in the presence of sulfur or chlorine or the co-existence of sulfur and chlorine, these sorbents were inactive. The effect of sulfur on Pb partitioning in the sludge incineration process mainly depended on the gas phase reaction, the surface reaction, the volatilization of products, and the concentration of Si, Ca and Al-containing compounds in the sludge. These findings provide useful information for understanding the partitioning behavior of Pb, facilitating the development of strategies to control the volatilization of Pb during sludge incineration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗