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DOE OSTI2022

Replication Data for: Hydrogen migration at restructuring palladium-silver oxide boundaries dramatically enhances reduction rate of silver oxide

The data underlying this published work have been made publicly available in this repository as part of the IMASC Data Management Plan. This work was supported as part of the Integrated Mesoscale Architectures for Sustainable Catalysis (IMASC), an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences under Award # DE-SC0012573.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Using a Chromatographic Pseudophase Model To Elucidate the Mechanism of Olefin Separation by Silver(I) Ions in Ionic Liquids

Silver(I) ions undergo selective olefin complexation and have been utilized in various olefin/paraffin separation techniques such as argentation chromatography and facilitated transport membranes. Ionic liquids (ILs) are solvents known for their low vapor pressure, high thermal stability, low melting points, and ability to promote a favorable solvation environment for silver(I) ion–olefin interactions. To develop highly selective separation systems, a fundamental understanding of analyte partitioning to the stationary phase and the thermodynamic driving forces behind solvation is required. In this study, a chromatographic model treating silver(I) ions as a pseudophase is constructed and employed for the first time to investigate the olefin separation mechanism in silver(I) salt/IL mixtures. Stationary phases containing varying amounts of noncoordinated silver(I) salt ([Ag + ][NTf 2 – ]) dissolved in the 1-decyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide ([C 10 MIM + ][NTf 2 – ]) IL are utilized to determine the partition coefficients of various analytes including alkanes, alkenes, alkynes, aromatics, aldehyde, esters, and ketones. As ligand coordination to silver(I) ions is known to lower its olefin complexation capability, this study also examines two different types of coordinated silver(I) ion pseudophases, namely, monocoordinated silver(I) salt ([Ag + (1-decyl-2-methylimidazole, DMIM)][NTf 2 – ]) and dicoordinated silver(I) salt ([Ag + (1-methylimidazole, MIM)(DMIM)][NTf 2 – ]). The extent of olefin partitioning to the coordinated silver(I) ion pseudophases over the carrier gas and IL decreased by up to two orders of magnitude. Values for enthalpy, entropy, and free energy of solvation were determined for the three silver(I) ion-containing systems. Olefin retention was observed to be enthalpically dominated, while ligand coordination to the silver(I) ion pseudophase resulted in variations for both enthalpic and entropic contributions to the free energy of solvation. Furthermore, the developed model can be used to study chemical changes that occur in silver(I) ions over time as well as identify optimal silver(I) salt/IL mixtures that yield high olefin selectivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2013

Method for Reduction of Silver Biocide Plating on Metal Surfaces

Silver ions in aqueous solutions (0.05 to 1 ppm) are used for microbial control in water systems. The silver ions remain in solution when stored in plastic containers, but the concentration rapidly decreases to non-biocidal levels when stored in metal containers. The silver deposits onto the surface and is reduced to non-biocidal silver metal when it contacts less noble metal surfaces, including stainless steel, titanium, and nickel-based alloys. Five methods of treatment of contact metal surfaces to deter silver deposition and reduction are proposed: (1) High-temperature oxidation of the metal surface; (2) High-concentration silver solution pre-treatment; (3) Silver plating; (4) Teflon coat by vapor deposition (titanium only); and (5) A combination of methods (1) and (2), which proved to be the best method for the nickel-based alloy application. The mechanism associated with surface treatments (1), (2), and (5) is thought to be the development of a less active oxide layer that deters ionic silver deposition. Mechanism (3) is an attempt to develop an equilibrium ionic silver concentration via dissolution of metallic silver. Mechanism (4) provides a non-reactive barrier to deter ionic silver plating. Development testing has shown that ionic silver in aqueous solution was maintained at essentially the same level of addition (0.4 ppm) for up to 15 months with method (5) (a combination of methods (1) and (2)), before the test was discontinued for nickel-based alloys. Method (1) resulted in the maintenance of a biocidal level (approximately 0.05 ppm) for up to 10 months before that test was discontinued for nickel-based alloys. Methods (1) and (2) used separately were able to maintain ionic silver in aqueous solution at essentially the same level of addition (0.4 ppm) for up to 10 months before the test was discontinued for stainless steel alloys. Method (3) was only utilized for titanium alloys, and was successful at maintaining ionic silver in aqueous solution at essentially the same level of addition (0.4 ppm) for up to 10 months before the test was discontinued for simple flat geometries, but not for geometries that are difficult to Teflon coat.

Steele, John↗

DOE OSTI2020

Characterizing Olefin Selectivity and Stability of Silver Salts in Ionic Liquids Using Inverse Gas Chromatography

Separation systems utilizing silver(I) ion-olefin complexation have limitations since silver(I) ions can be poisoned or reduced to metallic silver. Ionic liquids (ILs) are used as solvents for silver(I) ions to facilitate separations since their physico-chemical properties can be easily tuned. To develop separation systems with sustainable olefin selectivity, factors that affect silver(I) ion stability need to be understood. In this study, a total of 13 silver salt/IL mixtures were examined by inverse gas chromatography to identify the effects of silver salt anion and IL cation/anion combination on silver(I) ion stability. The effects of temperature and three different exposure gases on silver(I) ion stability were systematically studied. Exposing silver salt/IL mixtures to hydrogen at high temperatures had a greater effect on decreasing silver(I) ion-olefin complexation. Silver(I) ions from the silver bis[(trifluoromethyl)sulfonyl]imide ([NTf 2 – ]) salt were more stable in [NTf 2 – ]-containing ILs than in [BF 4 – ]-containing ILs. Optimum mixtures exhibited high olefin selectivity and were stable beyond 90 h when exposed to hydrogen gas.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Material Compatibility Study of Coated Metals to Maintain Biocidal Silver in a Spacecraft Potable Water System

Ionic silver-based biocide remains an option of choice for microbial control in spacecraft potable water systems. However, depletion of silver ions by wetted materials readily reduces ionic silver to nonbiocidal levels. This phenomenon occurs via various transport mechanisms at the liquid-solid interfaces between the silver-containing water and adjacent surfaces. Consequently, challenges remain in the design and/or selection of materials that can be used for the wetted system components that will help ensure silver is maintained at biocidal levels. Since silver has been baselined, and/or remains, as a potable water biocide option for several future spacecraft potable water systems, a multitiered approach is being investigated, looking at heritage materials, new processes, and/or alterative materials. This study conducted the application of eleven chemically-resistant coatings onto coupons that were cut out from three types of spacecraft-grade metals (Titanium Grade 2, Inconel 718, and 316L Stainless Steel) to investigate the performance of this material strategy as a barrier against silver depletion. In this investigation, the coated metals were immersed in a static 400 parts per billion silver biocide solution at a surface-area-to-volume ratio of 2.0 cm^(-1) and left to soak for predefined time periods. The concentration of the solution in contact with the coated samples was analyzed at various points via inductively coupled plasma mass spectrometry, and the measurements were interpreted as silver retention percentages over time. This paper summarizes the coating selection process, the configuration of the test, and the performance of each coating-metal combination at diminishing silver depletion. The preliminary results demonstrate that some of the selected coatings succeeded at maintaining biocidal silver concentrations far beyond the corresponding base metal in a similar test. The knowledge acquired through this investigation supports the deploying of coatings on plumbing lines for the integration of biocidal silver in the water system architecture of a spacecraft. Nevertheless, further testing must be continued to assess the performance of these coatings on other wetted geometries and any implications of unifying this material strategy with traditional and developmental engineering design processes for spacecraft potable water systems.

water↗

NASA NTRS2007

Assessment of Silver Based Disinfection Technology for CEV and Future US Spacecraft

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. As such, silver may reduce the overall complexity and mass of future spacecraft potable water systems, particularly those used to support long duration missions. A primary technology gap identified for the use of silver biocide is one of material compatibility. Wetted materials of construction are required to be selected such that silver ion concentrations can be maintained at biocidally effective levels. Preliminary data on silver biocide depletion rates in heritage spacecraft potable water system wetted-materials of construction has been gathered as part of a multi-phase test project aimed at the characterization of silver based biocide technology through: development of preferred materials lists, investigation of silver biocide forms and delivery methods, down-selection of silver biocide technologies, and integrated testing. A 10% - 20% loss in silver ion concentration per day was observed for acid passivated Nitronic 40 tubing with surface area to volume (S/V) ratios of approximately 4.59 cm-1. The Nitronic 40 tubes were tested both with and without biocide pretreatment. Silver biocide depletion was also observed at approximately 0.1% per day for the first 35 days of exposure to acid passivated Inconel 718 coupon, S/V of approximately 0.14 cm-1. Surface analysis by scanning election microscopy (SEM) suggested deposition of silver metal on both test materials. SEM analysis also provided evidence of potential variability in the passivation process for tube configuration of the Nitronic 40 test apparatus. These preliminary results are presented and discussed herein, along with the current project status.

Callahan, Michael R.↗

NASA NTRSDate not supplied

Feasibility Testing of Silver Electrolysis for Disinfection of Spacecraft Potable Water Systems

Anodic dissolution of silver electrodes, or “silver electrolysis,” is being investigated as a means of introducing biocidal silver into potable water on exploration spacecraft. A proof-of-concept prototype of a silver electrolysis reactor was developed, and feasibility was demonstrated for imparting a target silver concentration into a spacecraft water system. Prototype testing showed that the primary initial concerns related to the technology - inefficiencies of electrolysis in low conductivity water, the potential formation of resistive oxides on the electrode surfaces, and the potential for release of electrolytically-generated silver particles to the effluent water - were not problematic over the duration of the feasibility testing. The testing also demonstrated advantages of the technology, including the ability to consistently deliver silver at targeted concentrations and the ability to directly correlate the silver concentration to measurements of water conductivity. On the other hand, the reliability of the system has not yet been demonstrated. During prototype testing, intermittent periods of poor reactor performance manifested as a decrease in voltage accompanied by a decrease in silver output. It was determined that the cause of this behavior was silver-based deposits on inter-electrode wetted surfaces forming a conductive “bridge” between electrodes. Ongoing testing and refinement of the prototype reactor design seek to elucidate the root cause the bridging phenomenon and identify associated mitigation strategies. Once resolved, long-term performance testing is planned as part of continued development of the electrolytic silver dosing system.

Silver↗

NASA NTRS2024

Substrate Matters: Ionic Silver Alters Lettuce Growth, Nutrient Uptake, and Root Microbiome in a Hydroponics System

Ionic silver (Ag+) is being investigated as a residual biocide for use in NASA spacecraft potable water systems on future crewed missions. This water will be used to irrigate future spaceflight crop production systems. We have evaluated the impact of three concentrations (31 ppb, 125 ppb, and 500 ppb) of ionic silver biocide solutions on lettuce in an arcillite (calcinated clay particle substrate) and hydroponic (substrate-less) growth setup after 28 days. Lettuce plant growth was reduced in the hydroponic samples treated with 31 ppb silver and severely stunted for samples treated at 125 ppb and 500 ppb silver. No growth defects were observed in arcillite-grown lettuce. Silver was detectable in the hydroponic-grown lettuce leaves at each concentration but was not detected in the arcillite-grown lettuce leaves. Specifically, when 125 ppb silver water was applied to a hydroponics tray, Ag+ was detected at an average amount of 7 μg/g (dry weight) in lettuce leaves. The increase in Ag+ corresponded with a decrease in several essential elements in the lettuce tissue (Ca, K, P, S). In the arcillite growth setup, silver did not impact the plant root zone microbiome in terms of alpha diversity and relative abundance between treatments and control. However, with increasing silver concentration, the alpha diversity increased in lettuce root samples and in the water from the hydroponics tray samples. The genera in the hydroponic root and water samples were similar across the silver concentrations but displayed different relative abundances. This suggests that ionic silver was acting as a selective pressure for the microbes that colonize the hydroponic water. The surviving microbes likely utilized exudates from the stunted plant roots as a carbon source. Analysis of the root-associated microbiomes in response to silver showed enrichment of metagenomic pathways associated with alternate carbon source utilization, fatty-acid synthesis, and the ppGpp (guanosine 3′-diphosphate 5′-diphosphate) stringent response global regulatory system that operates under conditions of environmental stress. Nutrient solutions containing Ag+ in concentrations greater than 31 ppb in hydroponic systems lacking cation-exchange capacity can severely impact crop production due to stunting of plant growth.

lettuce↗

NASA NTRS2011

Disinfection of Spacecraft Potable Water Systems by Passivation with Ionic Silver

Microbial growth is common on wetted surfaces in spacecraft environmental control and life support systems despite the use of chemical and physical disinfection methods. Advanced control technologies are needed to limit microorganisms and increase the reliability of life support systems required for long-duration human missions. Silver ions and compounds are widely used as antimicrobial agents for medical applications and continue to be used as a residual biocide in some spacecraft water systems. The National Aeronautics and Space Administration (NASA) has identified silver fluoride for use in the potable water system on the next generation spacecraft. Due to ionic interactions between silver fluoride in solution and wetted metallic surfaces, ionic silver is rapidly depleted from solution and loses its antimicrobial efficacy over time. This report describes research to prolong the antimicrobial efficacy of ionic silver by maintaining its solubility. Three types of metal coupons (lnconel 718, Stainless Steel 316, and Titanium 6AI-4V) used in spacecraft potable water systems were exposed to either a continuous flow of water amended with 0.4 mg/L ionic silver fluoride or to a static, pre-treatment passivation in 50 mg/L ionic silver fluoride with or without a surface oxidation pre-treatment. Coupons were then challenged in a high-shear, CDC bioreactor (BioSurface Technologies) by exposure to six bacteria previously isolated from spacecraft potable water systems. Continuous exposure to 0.4 mg/L ionic silver over the course of 24 hours during the flow phase resulted in a >7-log reduction. The residual effect of a 24-hour passivation treatment in 50 mg/L of ionic silver resulted in a >3-log reduction, whereas a two-week treatment resulted in a >4-log reduction. Results indicate that 0.4 mg/L ionic silver is an effective biocide against many bacteria and that a prepassivation of metal surfaces with silver can provide additional microbial control.

Birmele, Michele N.↗

NASA NTRSDate not supplied

Early Results from a Broad Compatibility Study of Various Materials with Ionic Silver Biocide

Ionic silver is baselined for microbial control in spacecraft potable water systems forfuture exploration missions, but materials compatibility analysis is required to evaluate thepassive depletion of ionic silver concentration onto wetted material surfaces over time.Various articles concerning such testing have been published that examine interactions withwater containing ionic silver biocide, but most tests have focused on only a couple ofmaterials each and comparing results of different evaluations to one another has provedchallenging.This paper reports the first results from static exposure testing of a large arrayof material coupons to a 400 parts per billion (ppb) aqueous silver fluoride (AgF) solution,using a surface to volume ratio of approximately 2 cm-1. The test is designed in two mainstages. Stage 1 is a one-week screening to evaluate silver uptake. Materials that performmodestly to well after that week are promoted to Stage 2, which is a longer test with periodicsampling to examine the silver uptake rates over time; these samples are evaluated for otherwater quality parameters in addition to the remaining silver concentration. In a tangentialinvestigation, select materials that take up some silver in Stage 1 may be “aged” by repeatingthe Stage 1 test to determine whether repeated exposure reduces silver uptake rate, andsuccessfully aged materials may then continue to Stage 2 testing. The materials under testinclude metallic and polymeric materials with various surface finishes, treatments, andcoatings, as well as select other materials historically used in spacecraft water systems. Thistest began in August 2019, and thus only includes early results; future follow-on papers willinclude additional results as the test progresses. The ultimate goal builds a broad, easilycomparable data set that can be used to guide material selections for silver biocide-compatible spacecraft water system design.

Silver Biocide↗

NASA NTRS2014

Characterization of Electrochemically Generated Silver

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.

Adam, Niklas↗

NASA NTRS2018

Investigation of Silver Biocide as a Disinfection Technology for Spacecraft-An Early Literature Review

An ideal spacecraft water disinfection system should prevent or control microbial growth, inhibit or prevent biofilm formation, and prevent microbial-induced corrosion. In addition, the selected biocide system should be chemically compatible with materials used in the water storage and distribution system, have minimal maintenance requirements, especially for long-duration missions, and should be safe for crew consumption at levels appropriate for biocidal control. Silver ion is a proven broad spectrum biocide. There has been an increased interest in the biocidal function of silver, both due to its potential to control biocide resistant species and due to advances in silver and nanosilver biocide technologies. NASA is considering silver as the future biocide for exploration over the iodine biocide system. In order to select and design a successful silver biocide delivery system to meet NASA's requirements, it is essential to understand the advantages and disadvantages of moving to a silver disinfection system. To enhance the knowledge base for the application of silver biocides in spacecraft water systems, this paper provides a first compilation of review data related to: (1) Silver as a biocide technology, (2) Options and concepts for silver biocide delivery, and (3) Silver biocide compatibility studies for spacecraft systems.

Li, Wenyan↗

NASA NTRS2019

Silver Foam as Long-Term Passive Biocide for Potable Water Systems

A spacecraft water disinfection system, suitable for extended length space exploration missions, should prevent or control the growth of microbes, prevent or limit biofilm formation, and prevent microbiologically-influenced corrosion. In addition, the system should have minimal maintenance requirements, the effluent should be chemically compatible with all materials in contact with the water, be safe for human consumption, and suitable to be shared across international spacecraft platforms and mission architectures. Silver ions are a proven broad spectrum biocide. Silver is also the potable water biocide of choice for future exploration missions. Currently, the proposed method for implementing silver biocide in spacecraft systems relies on silver electrode technology to produce a controlled amount of silver ions. Unfortunately, electrolytic-based silver dosing presents multiple inherent challenges that affect performance and increase maintenance requirements over time. To decrease the risk of failure, an alternative silver biocide delivery method is needed. Control-release technology is an attractive option for developing a passive high-reliability silver dosing device. The concept of a nanoparticle/polyurethane (PU) composite foam for the controlled release of silver was prompted by the controlled release technology developed by NASA for the delivery of corrosion inhibitors and indicators. This paper presents the technical background and results from the synthesis and properties testing of the silver nanoparticles (AgNPs)/PU composite foam that is being developed for use in spacecraft potable water systems.

Irwin, Tesia D.↗

DOE OSTI2024

Recycling of silver from silicon solar cells by laser debonding

A laser-debonding approach to silver electrode recovery from solar cells is presented to address the critical need for efficient and eco-friendly recycling methods. The study explores the use of UV nanosecond and IR continuous-wave lasers to precisely debond silver electrodes from silicon wafers. By optimizing parameters like laser power, scan speed, and the number of passes, intact silver electrical contact lines were recovered from solar cells. Scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS) analysis confirmed the successful separation of silver from silicon wafers. Furthermore, an increase in the number of laser passes led to the production of silver microparticles, as validated by morphology and compositional studies using EDS. The estimated silver is approximately 90 mg for the Si solar cells of 15.4 * 15.4 cm 2 used in the study. To achieve a large area recovery of silver, a MATLAB code incorporating detection algorithms and specific criteria to automate laser scanning by accurately identifying the location of silver electrodes was developed. This presented laser debonding method is not confined to silicon solar cells but can be extended to other solar cell types featuring metal electrodes, offering a versatile solution. By minimizing the use of hazardous chemicals and reducing operational costs, the developed process aligns with the imperative of environmentally responsible photovoltaic waste management.

14 SOLAR ENERGY↗

NASA NTRSDate not supplied

Broad Compatibility Study of Polymeric Materials with Ionic Silver Biocide, Part I

NASA is considering ionic silver as a residual biocide for use in potable water systems being planned for future exploration spacecraft. Compatibility of the biocide with the system’s wetted-materials of construction remains a challenge. Due to the relatively inert nature of plastics, their use in varied water system applications may offer unique opportunities to address many biocide compatibility issues. A 2020 ICES paper described a “Stage 1” assessment of several polymeric materials, in which coupons having a 2 cm 1 surface to volume ratio were exposed to solutions of 400 parts per billion (ppb) aqueous silver fluoride (AgF) for one week. In this current paper, additional Stage 1 test results are presented for select epoxies and lubricants applied on silver-inert substrates. The coupon exposure studies were also expanded to a duration of 5 weeks for the “well-behaved” Stage 1 plastics previously reported: those exhibiting silver losses above 10% and less than 50%. For this type of Stage 2 testing, silver biocide solution samples are taken from three separate (and not previously-sampled) coupon containers after 3 days, and 2, 3, 4, and 5 weeks of exposure. "Very well-behaved" Stage 1 plastics will be tested in the same manner over one year, with longer sample intervals; early-period results are included here. In addition, for select materials, the coupons were “aged” by refilling test containers with fresh AgF and observing the respective silver uptake over similar Stage 2 test durations. For all test series, Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and ion-selective electrode (ISE) analyses were used to determine total and ionic silver (Ag+) concentrations, respectively. Additional sample analyses for Stage 2 tests includes total organic carbon (TOC), pH, conductivity, and oxidation-reduction potential (ORP). Ultimately, these early compatibility studies will be used to guide future material selections for developing silver biocide-compatible spacecraft water systems.

Silver Biocide↗

NASA NTRSDate not supplied

Material Compatibility Study of Coated Metals to Maintain Biocidal Silver in a Spacecraft Potable Water System

Ionic silver-based biocide is an option of strong interest for future exploration and has been baselined for several emerging spacecraft potable water systems. A challenge for the use of silver biocide remains the depletion of ionic silver on wetted materials of construction. Consequently, the design and/or selection of materials that can be used as the wetted system components need specific consideration. As part of the strategy to address this issue, a multitiered approach is being investigated that looks at combinations of conventional and non-conventional spacecraft treatment processes and materials. In this study, eleven chemically-resistant polymer coatings were applied as surface treatments onto coupons that were cut out from three types of conventional spacecraft-grade metals (Titanium Grade 2, Inconel 718, and 316L Stainless Steel). The coated metals were immersed in a static 400 parts per billion silver biocide solution at a surface-area-to-volume ratio of 2.0 cm^-1 and left to soak for predefined periods of time. The concentration of the solution in contact with the coated samples were then analyzed via inductively coupled plasma mass spectrometry, and the data used to determine the extent to which the coatings provided a barrier to silver loss. This paper summarizes the coating selection process, the configuration of the test, and the performance of each coating-metal combination as a mitigation to silver depletion. The preliminary results demonstrate that select coatings are proving effective at maintaining biocidal silver concentrations. The knowledge acquired through this investigation will be used to assess the feasibility of using these coatings as a robust strategy for maintaining biocidal silver in the water systems. Future studies are planned to assess the specific use of these coatings and to better understand the implications of utilizing this material approach in the future spacecraft potable water system designs.

coatings↗

NASA NTRSDate not supplied

Material Compatibility Study of Coated Metals to Maintain Biocidal Silver in a Spacecraft Potable Water System

coatings↗

DOE OSTI2023

Importance of the Heat Treatment Scheme on Self-Reducing Reactive Silver Inks

Self-reducing reactive silver inks can print high-quality silver at reasonable temperatures. While numerous studies have explored the impact of processing temperature on electrical properties, the role of the heat treatment scheme has not yet been studied. Common heat treatment schemes include printing and drying inks at room temperature before heat treatment, performing heat treatments while the inks are still wet, and directly printing the inks onto heated substrates. Each scheme generates distinct heat transfer and mass transport kinetics that can affect the silver morphology and electrical properties. However, to date, the impact of different schemes has not been systematically investigated. To address this knowledge gap, this work investigates how different heat treatment schemes impact metal formation, sintering, and the resultant electrical properties of printed self-reducing reactive silver inks. Heat treatment on room-temperature dried inks and wet inks, with top-down (oven) and bottom-up (hot plate) heating sources, were compared. Inks dried at room temperature resulted in extremely porous films that required high heat treatment temperatures (>100 °C) for silver densification. However, these dried films could only densify locally, and their high initial porosities resulted in voids and high resistances (~0.6 Ω mm –1 ) even after heat treatments above 300 °C. Inks that were wet during heat treatment showed moderate improvements in electrical properties with resistances on the order of 0.4 Ω mm –1 at heat treatments of 250 °C. Printing reactive inks directly onto heated substrates yielded the best low-temperature results, with 0.46 Ω mm –1 (5.5 × bulk silver) line resistances achieved at only 90 °C. Overall, this work’s experimental results provide detailed insights into why printing onto a heated substrate results in superior electrical performance compared to more common heat treatment schemes. Additionally, controlling where the precipitation reaction occurs is critical to controlling the film morphology and properties. As a result, this work shows that even an ammonia-based silver reactive ink can achieve good, low-temperature electrical properties with the proper heat treatment scheme.

14 SOLAR ENERGY↗