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Temperature rise of micron sized silver particles on carbon film due to electron beam heating, setting up heat balance equation
Particles from a variety of silver powders were investigated by scanning electron microscopy and particle size analyses. Particle size distribution curves and volume population graphs were prepared for these silver powders and for glass powders with optimum, extra fine and coarse particle sizes. The viscosity at a given shear rate and slope of viscosity over a range of shear rates were determined for thick film pastes made with these powders. Because of particle anomalies and variations, the need for flexibility to achieve the best printing qualities for silver pastes was evident. It was established that print quality, dried and fired film density and optimum contact of silver particles with silicon, important for cell electrical output, could be achieved by adjusting the slope of viscosity that fell outside of the range, -0.550 to -0.650. This was accomplished through organic vehicle technology that permitted a change in the slope of viscosity, up or down, while maintaining a constant silver and total solids content.
The high spectral and spatial resolution thermal infrared (TIR) data to be acquired from the upcoming Mars Observer-Thermal Emission Spectra (TES) mission will map the composition and texture of the Martian sediments. To prepare for these data, portions of two remote sensing experiments were conducted to test procedures for extracting surface property information from TIR data. Reported here is the continuing analysis of Thermal Infrared Multispectral Scanner (TIMS) data, field emission spectra, laboratory Fourier Transform Infrared (FTIR) reflectance spectra, and field observations with respect to the physical characteristics (composition, emissivity, etc.) of Silver Lake playa in southern California.
Silver biocide offers a potential advantage over iodine, the current state of the art in US spacecraft disinfection technology, in that silver can be safely consumed by the crew. Low concentrations of silver (<500 ppb) have been shown to kill bacteria in water systems and keep it safe for potability. Silver does not require hardware to remove it from a water system, and therefore can provide a simpler means for disinfecting water. The Russian segment of the International Space Station has utilized an electrochemically generated silver solution, which is colloidal in nature. To be able to reliably provide a silver biocide to drinking water by electrochemical means would reduce mass required for removing another biocide such as iodine from the water. This would also aid in crew time required to replace iodine removal cartridges. Future long term missions would benefit from electrochemically produced silver as the biocide could be produced on demand and requires only a small concentration to be effective. Since it can also be consumed safely, there is less mass in removal hardware and little consumables required for production. The goal of this project initially is to understand the nature of the electrochemically produced silver, the particle sizes produced by the electrochemical cell and the effect that voltage adjustment has on the particle size. In literature, it has been documented that dissolved oxygen and pH have an effect on the ionization of the electrochemical silver so those parameters would be measured and possibly adjusted to understand their effect on the silver.
We report catalysts have been prepared on a low surface area α-Al 2 O 3 support used commercially for previous generation olefin epoxidation catalysts. Prescreening of the low surface area alumina (0.73 m 2 /g) indicated the absence of acid catalyzed isomerization of EO at an evaluation temperature of 210 °C. A 0.1 wt% Ag base material synthesized by incipient wetness impregnation of AgNO 3 was used as a base material for electroless deposition (ED) of additional Ag to increase particle sizes by controlled reduction of Ag + directly onto the preexisting Ag surface to form weight loadings between 0.3 and 5.0 wt% metal. A 12 wt% Ag/α-Al 2 O 3 using Ag 2 C 2 O 4 as the Ag precursor was also prepared to compare performance of the ED samples with a catalyst more typical of industrial formulations. Characterization by SEM, STEM, and hydrogen titration of oxygen precovered Ag characterized before and after catalytic evaluation indicated that microscopy is required to accurately represent distributions of Ag particle sizes, but H 2 titration of O-precovered Ag gives the best representation of active sites since it directly counts the number of Ag surface sites. Larger particles >100 nm are resistant to both Ag sintering and carbon foulant; TOF values were relatively insensitive to particle size with only a 2.2 × difference between the best and worst performing samples. Selectivity, which is not a function of TOF, shows the most significant structure sensitivity effect where particle sizes follow the trend 67 nm ≈ 92 nm (58% EO) < 157 nm (67% EO) < 211–542 nm (73% EO). The lower EO selectivities were also correlated with increased fouling for the smaller Ag sizes, suggesting that more strongly bound EO precursor(s) leads to combustion and CO 2 /H 2 O formation.
Silver nanoparticles (NPs) are extensively used in electronic components, chemical sensors, and disinfection applications, in which many of their properties depend on particle size. However, control over silver NP size and morphology still remains a challenge for many synthesis techniques. Here, in this work, we demonstrate the surfactant-free synthesis of silver NPs using a low-pressure inductively coupled nonthermal argon plasma. Continuously forming droplets of silver nitrate (AgNO 3 ) precursor dissolved in glycerol are exposed to the plasma, with the droplet residence time being determined by the precursor flow rate. Glycerol has rarely been studied in plasma-liquid interactions but shows favorable properties for controlled NP synthesis at low pressure. We show that the droplet residence time and plasma power have strong influence on NP properties, and that improved size control and particle monodispersity can be achieved by pulsed power operation. Silver NPs had mean diameters of 20 nm with geometric standard deviations of 1.6 under continuous wave operation, which decreased to 6 nm mean and 1.3 geometric standard deviation for pulsed power operation at 100 Hz and 20% duty cycle. We propose that solvated electrons from the plasma and vacuum ultraviolet (VUV) radiation induced electrons produced in glycerol are the main reducing agents of Ag + , the precursor for NPs, while no significant change of chemical composition of the glycerol solvent was detected.
An investment casting process has been developed to produce net-shape, superconducting ceramics. In this work, a factorial experiment was performed to determine the critical process parameters for producing cast YBa2Cu3O7 ceramics with optimum properties. An analysis of variance procedure indicated that the key variables in casting superconductive ceramics are the particle size distribution and sintering temperature. Additionally, the interactions between the sintering temperature and the other process parameters (e.g., particle size distribution and the use of silver dopants) were also found to influence the density, porosity, and critical current density of the fired ceramics.
Experiments have shown the stability enhancement of polymeric sensing films on mixing the polymer with colloidal filler particles (submicron-sized) of carbon black, silver, titanium dioxide, and fumed silicon dioxide. The polymer films are candidates for potential use as sensing media in micro/nano chemical sensor devices. The need for stability enhancement of polymer sensing films arises because such films have been found to exhibit unpredictable changes in sensing activity over time, which could result in a possible failure of the sensor device. The changes in the physical properties of a polymer sensing film caused by the sorption of a target molecule can be measured by any of several established transduction techniques: electrochemical, optical, calorimetric, or piezoelectric, for example. The transduction technique used in the current polymer stability experiments is based on piezoelectric principles using a quartz-crystal microbalance (QCM). The surface of the QCM is coated with the polymer, and the mass uptake by the polymer film causes a change in the oscillating frequency of the quartz crystal. The polymer used for the current study is ethyl cellulose. The polymer/ polymer composite solutions were prepared in 1,3 dioxolane solvent. The filler concentration was fixed at 10 weight percent for the composites. The polymer or polymer composite solutions were cast on the quartz crystal having a fundamental frequency of about 6 MHz. The coated crystal was subjected to a multistage drying process to remove all measurable traces of the solvent. In each experiment, the frequency of oscillation was measured while the QCM was exposed to clean, dry, flowing air for about 30 minutes, then to air containing a known concentration of isopropanol for about 30 minutes, then again to clean dry air for about 30 minutes, and so forth. This cycle of measurements for varying isopropanol concentrations was repeated at intervals for several months. The figure depicts some of the sensing film stability results for ethyl cellulose polymer, ethyl cellulose-carbon black, and ethyl cellulose-silicon dioxide composite systems. An ethyl cellulose film exhibited a marked decline in response in the first few months of study and settled to a steady average response after about four months. However, response varied widely around the average response for ethyl cellulose film. In contrast, ethyl cellulose- carbon black and ethyl cellulose-silicon dioxide composites also declined in the early months, but showed more repeatable sensing film activity after the initial decline. Similar trends were observed in experiments for ethyl cellulose-titanium dioxide and ethyl cellulose-silver composites.
Uniform and nonuniform size and energy glass bead and silver alloy and aluminum powder particles effects on sediment volume and viscosity in propylene oxide and mineral oil
Madidrop is a rectangular ceramic tablet originally designed to dose a 10-20-liter volume of water with silver to act as a biocide for remote communities with unreliable water sources. Silver as a biocide is a proposed method to control bacteria on the International Space Station or future Artemis missions. This would replace iodine currently used due to issues with a dual biocide system in place between Russian and US segments and the extra cost of iodine removal required before consumption. NASA has been reviewing this Madidrop technology and its potential application with a water reclamation system on orbit to dose silver after purifying the water. While there are a couple alternative methods to dosing silver on station, this method is like the existing passive dosing method used currently to dose iodine. Tests conducted characterize the manufacturer’s original intent to leave the tablet in a tank for a specified amount of time before removing and testing alternative passive flow-through methods. Passive flow testing involved two options: keeping the tablet intact or crushing the tablet into smaller particle sizes to increase the surface area while varying particle sizes. The results of these tests revealed a large amount of silver output at first that quickly reduced to a constant lower output within a reasonable dosing concentration range. The initial high concentration peaks after a couple days of quiescence and could be useful for shocking the initial tank water contents. Madidrop used as a passive particle doser could act as a stand-in replacement for iodine in future spaceflight water reclamation systems.
Madidrop is a rectangular ceramic tablet originally designed to dose a 10-20-liter volume of water with silver to act as a biocide for remote communities with unreliable water sources. Silver as a biocide is a proposed method to control bacteria on the International Space Station or future Artemis missions. This would replace iodine currently used due to issues with a dual biocide system in place between Russian and US segments and the extra cost of iodine removal required before consumption. NASA has been reviewing this Madidrop technology and its potential application with a water reclamation system on orbit to dose silver after purifying the water. While there are a couple alternative methods to dosing silver on station, this method is like the existing passive dosing method used currently to dose iodine. Tests conducted characterize the manufacturer’s original intent to leave the tablet in a tank for a specified amount of time before removing and testing alternative passive flow-through methods. Passive flow testing involved two options: keeping the tablet intact or crushing the tablet into smaller particle sizes to increase the surface area while varying particle sizes. The results of these tests revealed a large amount of silver output at first that quickly reduced to a constant lower output within a reasonable dosing concentration range. The initial high concentration peaks after a couple days of quiescence and could be useful for shocking the initial tank water contents. Madidrop used as a passive particle doser could act as a stand-in replacement for iodine in future spaceflight water reclamation systems.
The Savannah River Site (SRS) produced tritium, plutonium, and special nuclear materials for national defense, medicine, and the space programs. As part of operations, the F-Area Seepage Basins operated until 1988 for the disposition of deionized acidic wastewater from the F Separations Facility. The wastewater contained dilute nitric acid and low concentrations of non-radioactive metals, and radionuclides, with the major isotopes being Cs-137, Sr-90, U-235, U-238, Pu-239, Tc-99, I-129, and tritium. The seepage basins were closed in 1988 and backfilled and capped by 1991. The groundwater emanating from beneath the closed and capped seepage basins is acidic and contains elevated levels of both chemical and radiological contaminants. Releases from the groundwater plumes sourced from the F-Area Seepage Basins have impacted the water quality of Fourmile Branch, which is a small tributary to the Savannah River, a regional water source. A large pump-and-treat system was constructed in 1997 and operated until 2003 in an attempt to capture the releases to Fourmile Branch. The system in F Area and a similar system in H Area were expensive (∼$1.3 M/month) to operate and produced large quantities of radioactive waste, with concentrations of I- 129 too high to be disposed of at the SRS. In 2004, SRS replaced pump-and-treat with a funnel and gate system that along with operation of a base injection system at the gates reduces the flux of contaminants to the wetlands adjacent to Fourmile Branch. The alkaline solution injected into the aquifer neutralizes the acidic plume and immobilizes many of the cationic constituents. However, base injection is not effective in managing the release of iodine-129, an anionic contaminant. To address iodine-129 SRS and the Savannah River National Laboratory developed an in situ technology that uses ultra-fine ground silver chloride (AgCl) as an injectable capture medium for the sequestration of iodine-129. The AgCl amendment has a very small particle size and is designed to be injected into the contaminated aquifer to capture iodine-129. Dissolved iodine-129 forms a stable and highly insoluble solid (silver iodide) upon contact with AgCl. Laboratory studies, a field scale pilot test (2009), and three deployments (2011, 2015 and 2019) of AgCl have been successfully performed at the F-Area Seepage Basins. (authors)
The work described herein assesses the ability to characterize gold nanoparticles (Au NPs) of 50 and 100 nm, as well as 60 nm silver shelled gold core nanospheres (Au/Ag NPs), for their mass, respective size, and isotopic composition in an automated and unattended fashion. Here, an innovative autosampler was employed to mix and transport the blanks, standards, and samples into a high-efficiency single particle (SP) introduction system for subsequent analysis by inductively coupled plasma–time of flight–mass spectrometry (ICP-TOF-MS). Optimized NP transport efficiency into the ICP-TOF-MS was determined to be >80%. This combination, SP-ICP-TOF-MS, allowed for high-throughput sample analysis. Specifically, 50 total samples (including blanks/standards) were analyzed over 8 h, to provide an accurate characterization of the NPs. This methodology was implemented over the course of 5 days to assess its long-term reproducibility. Impressively, the in-run and day-to-day variation of sample transport is assessed to be 3.54 and 9.52% relative standard deviation (%RSD), respectively. The determination of Au NP size and concentration was of <5% relative difference from the certified values over these time periods. Isotopic characterization of the 107 Ag/ 109 Ag particles (n = 132,630) over the course of the measurements was determined to be 1.0788 ± 0.0030 with high accuracy (0.23% relative difference) when compared to the multi-collector–ICP-MS determination.
The sintering processing–structure–property relationship of a multiscale silver materials is investigated: microparticles with nanofeatures, particularly on their three-dimensional (3D) morphology. The target application is to replace conventional lead-based solders in advanced electronic manufacturing. Unlike lead-based solders, silver powders are suited to satisfy increasingly demanding mechanical, electrical, and thermal requirements, meanwhile being free of health effect. Sintering the material at a low temperature and without applied pressure are desirable conditions, which results in a preferred use of silver nanoparticles, as nanofeatures have higher driving force to sinter with the decrease in particle size. However, nanosized powders present potential health/environmental effects. To address the trade-off between the benefits and shortcomings of nano-versus microparticles, this work studies a novel multiscale silver paste, namely micron-sized powders with nanosized features. To get quantitative 3D visualization of micro- and nanoscale features, ptychographic X-ray computed nanotomography is applied. The correlations between conditions (thermal aging, pressure, and substrate metallization), mechanical properties, and morphological parameters are established. Finally, using novel 3D X-ray nanoimaging technique, it is demonstrated that one can design multiscale materials while balancing complex demands required in advanced electronics manufacturing and research directions in materials design and characterization.
The effects of BaF2-CaF2 particle size and size distribution on PS304 feedstock powder flowability have been investigated. Angular BaF2-CaF2 eutectic powders were produced by comminution and classified by screening to obtain 38 to 45 microns 45 to 106 microns, 63 to 106 microns, 45 to 53 microns, 63 to 75 microns, and 90 to 106 microns particle size distributions. The fluorides were added incrementally from 0 to 10 wt% to the other powder constituents of the PS304 feedstock: nichrome, chromia, and silver powders. The flow rate of the powder blends decreased linearly with increasing concentration of the fluorides. Flow was degraded with decreasing BaF2-CaF2 particle size and with increasing BaF2-CaF2 particle size distribution. A semiempirical relationship is offered to describe the PS304 powder blend flow behavior. The Hausner Ratio confirmed the funnel flow test results, but was slightly less sensitive to differences in BaF2-CaF2 particle size and size distribution. These findings may have applicability to other powders that do not flow easily, such as ceramic powders.
A superconductor, of composition Y(Ba,K,Na)2Cu3O(x)/F(y) and a composite of composition Y(Ba,K,Na)2Cu3O(x)/F(y) + Ag, with changing K, Na and F content but a constant silver content (Ag = 10 mass%) was prepared using a single heat treatment. the resulting material was ground in a corundum lined mill, separated to particle size fractions of 0-40 micron, 0-63 micron and 63-900 micron and explosively compacted, using an explosive pressure of 10(exp 4) MPa and a subsequent heat treatment. Best results were obtained with the 63-900 micron fraction of composition Y(Ba(1.95) K(0.01)Cu3O(x)F(0),(05)/Ag: porosity less than 0.01 cu cm/g and current density 2800 A/sq cm at 77K.
Nitric and hydrochloric acids have been postulated to condense in the winter polar stratosphere to become an important component of polar stratospheric clouds. One implication is that the removal of NO(y) from the gas phase by this mechanism allows high Cl(x) concentrations to react with O3, because the formation of ClNO3 is inhibited. Contributions of NO3 and Cl to the stratospheric aerosol were determined during the 1987 Airborne Antarctic Ozone Experiment by testing for the presence of nitrates and chlorides in the condensed phase. Aerosol particles were collected on four 500 micron diameter gold wires, each pretreated differently to give results that were specific to certain physical and chemical aerosol properties. One wire was carbon-coated for concentration and size analyses by scanning electron microscopy; X-ray energy dispersive analyses permitted the detection of S and Cl in individual particles. Three more wires were coated with Nitron, barium chloride and silver nitrate, respectively, to detect nitrate, sulfate and chloride in aerosol particles. All three ions, viz., sulfates, nitrates and chlorides were detected in the Antarctic stratospheric aerosol. In terms of number concentrations, the aerosol was dominated by sulfates, followed by chlorides and nitrates. An inverse linear regression can be established between nitrate concentrations and ozone mixing ratio, and between temperature and nitrates.
Plasmon induced hot carrier transfer is a promising novel approach for solar energy conversion, but its practical application is often hindered by its low efficiency. This work demonstrates an unprecedented quantum efficiency of plasmonic hot-electron transfer of up to 53 ± 2% from 1.7 nm silver nanoparticles to anatase nanoporous TiOsub>2 films at 400 nm excitation. This efficient hot-electron transfer consists of contributions of both hot electrons generated by plasmon decay through exciting Ag intraband transitions and Ag-to-TiO 2 interfacial charge-transfer transitions. The efficiencies of both pathways increase at smaller Ag particle sizes from 5.9 to 1.7 nm, suggesting that decreasing particle sizes is a promising way toward efficient plasmonic hot-carrier extraction.