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At least 235 records · Page 13

Electrochemical Investigation of Moisture Byproducts in Molten Calcium Chloride

Residual water in molten CaCl 2 reacts to form different byproducts, such as HCl, which can impact the corrosivity of the salt and efficiency of electrochemical operations, such as electrolytic oxide reduction and electrorefining. The ability to detect and quantify these byproducts electrochemically can provide feedback on the efficacy of vacuum drying and other purification methods, as well as the impact of these byproducts on process operations. An electrochemical signal’s association with the production of H 2 is verified and characterized using cyclic voltammetry (CV) and residual gas analysis. CV estimated a 2-electron exchange process associated with H 2 production. CV detected trace quantities of an oxidized species containing hydrogen in the salt on the order of 10 ppm. Different salt handling methods were compared for their impact on the hydrogen electrochemical signal. It was found that 30 min of exposure of CaCl 2 in a beaker to low-humidity air (<20%) had minimal impact on the H 2 production signal.

Electrochemistry↗

PERMEABILITY TESTING OF SIMULATED SALTSTONE CORE AND VAULT 4 CELL E SALTSTONE

The Engineering Process Development Group (EPD) of the Savannah River National Laboratory (SRNL) prepared simulated saltstone core samples to evaluate the effect of sample collection by coring on the permeability of saltstone. The Environmental Restoration Technology Section (ERTS) of the SRNL was given the task of measuring the permeability of cores of simulated saltstone. Saltstone samples collected from Vault 4 Cell E using both dry and wet coring methods were also submitted for permeability analysis. The cores from Vault 4 Cell E were in multiple pieces when they were recovered (Smith, 2008 Cheng et.al, 2009). Permeability testing was only performed on the portions of the core sample that were intact, had no visible fractures or cracks, and met the specifications for 'undisturbed specimens' identified in Method ASTM D5084-03 Standard Test Methods for Measurement of Hydraulic Conductivity of Saturated Porous Materials Using a Flexible Wall Permeameter that was used for the testing. Permeability values for cores of simulated saltstone compared with values from permeability tests conducted on molded saltstone samples by an independent laboratory using the same method. All hydraulic conductivity results for Vault 4 samples exceeded results for both molded and cored saltstone simulant samples. The average hydraulic conductivity result for Vault 4 Cell E samples of 3.9 x 10{sup -7} cm/sec is approximately two orders of magnitude greater than that of the simulated saltstone with an average of 4.1 x 10{sup -9} cm/sec. Numerical flow and transport simulations of moisture movement through saltstone performed for the performance assessment of the Saltstone Disposal Facility (SDF) used 2.0 x 10{sup -9} cm/sec for the hydraulic conductivity of saltstone (Flach et al, 2009). The results for simulated versus actual saltstone were further compared using non-parametric statistics. The results from non-parametric statistical analysis of results indicate that there is at least a 98% probability that the hydraulic conductivity of saltstone samples collected from Vault 4 Cell E saltstone is greater than that of the baseline simulant mix.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

The SURE House (Solar Decathlon 2015)

Coastal towns and cities across the Northeastern US, with their high population density, aged utility infrastructure, and unique geography, are increasingly vulnerable to climate change related storm events. In October 2012 superstorm Sandy highlighted the fragility of our current coastal building types and made clear the need for a new model of design and construction which works to understand and mitigate these weaknesses. Dramatic changes in public policy, championed by both The Federal Emergency Management Agency (FEMA) and the National Flood Insurance Program (NFIP) are driving the rebuilding of these shore communities, often resulting in costly renovations, un-sustainable neighborhood configurations and in direct conflict with concurrent government policies such as The American with Disabilities Act (ADA). The SURE HOUSE demonstrates a series of new design solutions to these conflicting public policies and environmental imperatives. At Stevens Institute of Technology, the 2015 Solar Decathlon started with the challenge: Can we design a home for coastal New Jersey that dramatically reduces its energy use while protecting itself from the realities of a changing, more extreme climate? The SURE HOUSE merges the iconic 20th century shore home with 21st century building science. Utilizing innovative renewable energy technologies, a ‘Passive House’ level building envelope, and rugged glass-fiber-composite materials to flood-proof the home, the SURE HOUSE is a high-performance, net-zero-energy home, armored against extreme weather, designed for the contemporary lifestyle of the Jersey Shore and other vulnerable coastal communities. SUSTAINABLE At Stevens, we recognize that energy use in the home and workplace is directly connected to the growing problem of climate change. Reducing our energy consumption by designing higher performing, compact homes that are both functional, comfortable and desirable is the first critical step towards a modern, sustainable architecture for New Jersey and beyond. This is what informed the architectural design of the house. Configured about a compact form, thickly insulated and air-sealed walls eliminate thermal bridging and minimize energy losses while advanced glazing brings in free solar heat during the winter months. As a result of these passive design strategies, the SURE HOUSE has a greatly reduced carbon footprint requiring 91% less energy than a typical New Jersey home. Photovoltaic (PV) arrays on both the rooftop and operable shutters easily provide energy in excess of the home’s modest demands. The Stevens team considers a truly sustainable home in the era of climate change, one that prioritizes low energy use, and integrates right-sized renewable generation to supply the home’s needs. Low consumption, low production. RESILIENT In October of 2012, Hurricane Sandy wreaked havoc along the east coast of the US. In New Jersey alone there was an estimated 29.4 billion dollars in damages, 346,000 homes affected, and almost two and a half million people left without power, in some cases for over 10 days. Recovery from this storm and associated flooding is ongoing to this day, as many New Jersey homeowners grapple with the large costs of rebuilding and struggle to adapt to complicated new home building regulations. Damage from this storm to Hoboken, the home of the Stevens Institute of Technology’s campus, and to the New Jersey shore was extensive and many students on the SURE HOUSE team were directly affected by this historic event. The Stevens design team recognizes that in a world of more frequent and stronger storms, the ability to absorb and adapt to change is more important than ever. Successfully weathering the next storm and its aftermath is one of the primary goals in the design of the SURE HOUSE prototype. The SURE HOUSE introduces unique ‘dry flood-proofing’ methods to residential construction. Innovative wall and floor flood-proofing, utilizing durable composite sheathing materials adapted from the boating industry, were developed by the student team to render the SURE House’s building envelope flood proof up to the FEMA AE 6/7 Zone (+ 6/7 feet of water above sea-level). Designed and fabricated utilizing glass-fiber composite materials, the custom storm shutter system serves to protect the large glazed openings of the home from both air-borne debris impact and water infiltration during a storm event while also providing deterrence from the vandalism that often occurs in the aftermath of a calamitous event. During extended power outages, a ‘resilient’ solar array is capable of supplying critical amounts of energy and hot water to the home, without the use of battery storage or grid infrastructure. PV Description AC GRID-TIED PV SYSTEM The SURE HOUSE solar system consists of two distinct arrays, the grid-tied rooftop array which produces AC Powerand the shutter-mounted array which converts DC power generated by the modules directly into usable heat for the domestic hot water (DHW). The roof-mounted AC grid-tied array is comprised of three strings, two 11 module strings connected to an SMA SB 5000TL-US-223 inverter and a single 10 module string equipped and an SMA SB 3000TL-US-22 central inverter. All modules for the rooftop AC array are LG MonoX 2804 watt solar panels, chosen for their durability and efficiency. Inverter sizing and string size are optimized to the electrical characteristics of the chosen PV modules and the desired energy production, see Appendix 5B. The SURE HOUSE is projected to produce 12,353 kWh per year to meet 6,157 kWh per year of estimated consumption. Solar modules for the two AC grid-tied sub arrays are mounted on the main roof surface of the SURE HOUSE with a 10 degree tilt angle using a partially-ballasted polyethylene roof mounting system made by Renusol, which is particularly suited to the corrosive salt air of a coastal environment. This method was chosen for its installation simplicity and to limit detrimental roof penetrations. The 10 degree tilt optimizes the energy generated per roof area at a lower price, see Appendix 5A, and ensures that there is minimal wind uplift. DC SOLAR ELECTRIC DOMESTIC HOT WATER The SURE HOUSE’s approach to sustainable and resilient domestic hot water (DHW) consists of a unique, custom engineered DC solar electric hot water system. Employing the use of Advanced Energy’s DC electric PV heater (DCPVH)5 to heat domestic water well beyond the draw temperature, the SURE HOUSE is able to obtain a remarkably high solar fraction of 75% or more. The custom modified 80 gallon Vaughn DHW tank acts as a large solar ‘battery’ that stores heat energy in the form of hot water at almost 150 degrees, harvesting energy when the sun is out for use later in the day or overnight. The system, which uses electricity rather than heated fluid, is distinct from traditional ‘solar thermal’ systems by eliminating the dangers and associated maintenance issues of fluid based systems. By forgoing the use of external fluid loops, overheated solar collectors and pipes are not an issue for the SURE HOUSE system which never needs any yearly or seasonal flushing. In weather conditions where the integrated DCPVH unit cannot produce enough hot water via solar energy alone, the Vaughn hot water tank comes factory made with an AC powered 2.6 COP heat pump and a AC heating coil that serve as back-up heating elements. The DCPVH is powered by a DC array consisting of 10 custom-made Solbian by PVilion 180 watt, monocrystalline, flexible solar modules6. The Solbian modules are directly mounted to the top half of the operable storm shutters on the south façade of the SURE HOUSE. The SURE HOUSE team worked closely with PVillion, a PV system designer specializing in flexible architectural photovoltaics, to design an adhesive system that works with the glass-fiber storm shutter surface in a reliable manner over an extended period. Because this system operates in DC-only mode and never connects to the municipal power grid, the system can continue to create hot water safely and effectively even during grid disruption events. This hot water, and the energy stored within it, could be used for a range of activities including washing and cooking to more elaborate hydronic heating systems as desired. See Appendix 6 for system engineering, sizing and modeling.

14 SOLAR ENERGY↗

County-level Estimates for Carbon Distribution in U.S. Croplands, 1990-2005

Net Primary Productivity (NPP) for croplands can be estimated using a statistical method that includes factors for dry weight, harvest indices, and root:shoot ratios multiplied by yield data from the National Agricultural Statistics Service (NASS). This method has been documented and published by Prince et al. (2001), Hicke and Lobell (2004), and Hicke et al. (2004). We expanded this method by including factors for more crops and by using an estimated carbon content of 0.45 for agricultural crops to estimate (a) total net carbon uptake, (b) carbon in aboveground biomass, (c) carbon in belowground biomass, (d) carbon harvested and transported off site, and (e) the amount of carbon remaining on the surface following harvest. These five variables are included with their respective Federal Information Processing Standards (FIPS) codes for all counties in the contiguous U.S. from 1990-2005. A mean harvest efficiency of 0.95 was assumed across all crops. Total cropland NPP for the U.S. ranges from 378-527 Tg C yr-1 within years 1990-2005, and total carbon harvested and removed ranges from 161-228 Tg C yr-1 within years 1990-2005.For access to the data files, click this link to the CDIAC data transition website: http://cdiac.ess-dive.lbl.gov/carbonmanagement/cropcarbon/

54 ENVIRONMENTAL SCIENCES↗

Dry Sintered Metal Coating of Halloysite Nanotubes

Halloysite nanotubes (HNTs) are a naturally-occurring aluminosilicate whose dimensions measure microns in length and tens of nanometers in diameter. Bonding defects between the alumina and silica lead to net negative and positive charges on the exterior and interior lumen, respectively. HNTs have been shown to enhance the material properties of polymer matrices and enable the sustained release of loaded chemicals, drugs, and growth factors. Due to the net charges, these nanotubes can also be readily coated in layered-depositions using the HNT exterior lumen’s net negative charge as the basis for assembly. These coatings are primarily done through wet chemical processes, the majority of which are limited in their use of desired chemicals, due to the polarity of the halloysite. Furthermore, this restriction in the type of chemicals used often requires the use of more toxic chemicals in place of greener options, and typically necessitates the use of a significantly longer chemical process to achieve the desired coating. In this study, we show that HNTs can be coated with metal acetylacetonates—compounds primarily employed in the synthesis of nanoparticles, as metal catalysts, and as NMR shift reagents—through a dry sintering process. This method was capable of thermally decaying the metal acetylacetonate, resulting in a free positively-charged metal ion that readily bonded to the negatively-charged HNT exterior, resulting in metallic coatings forming on the HNT surface. Our coating method may enable greater deposition of coated material onto these nanotubes as required for a desired application. Moreover, the use of chemical processes using toxic chemicals is not required, thus eliminating exposure

36 MATERIALS SCIENCE↗

Toward Interpreting Failure in Sintered-Silver Interconnection Systems

The mechanical strength and subsequent reliability of a sintered-silver interconnection system is a function of numerous independent parameters. That system is still undergoing process development. Most of those parameters (e.g., choice of plating) are arguably and unfortunately taken for granted and are independent of the silver s cohesive strength. To explore such effects, shear strength testing and failure analyses were completed on a simple, mock sintered-silver interconnection system consisting of bonding two DBC ceramic substrates. Silver and gold platings were part of the test matrix, as was pre-drying strategies, and the consideration of stencil-printing vs. screen-printing. Shear strength of sintered-silver interconnect systems was found to be was insensitive to the choice of plating, drying practice, and printing method provided careful and consistent processing of the sintered-silver are practiced. But if the service stress in sintered silver interconnect systems is anticipated to exceed ~ 60 MPa, then the system will likely fail.

Wereszczak, Andrew A↗

Method of fracking using silicone surfactants

Methods for fracking, particularly dry fracking, comprising the use of surfactants for preparation of substantially water-free carbon dioxide in oil foams are presented.

02 PETROLEUM↗

Electrical capacitance as a predictor of root dry weight in shrub willow ( Salix ; Salicaceae) parents and progeny

Premise of the study: Root biomass is an important trait often disregarded in woody perennial selection due to the challenge and expense of accurately and efficiently measuring large populations. In this study, we aim to develop a simple method that can predict root dry weight within a diverse shrub willow ( Salix ) breeding population representing species hybrids and their parents using root electrical capacitance (REC). Methods: The REC method was tested on plants started from cuttings and grown in pots with potting mix in the greenhouse for 11 wk to assess the relationship of REC with 24 biomass traits and its usefulness in allometric models for root and stem dry biomass. Results: Strong linear and positive correlations were found between REC and root dry biomass ( r = 0.88). The total proportion of variance of root and stem dry biomass explained by predictors in multiple regression was 85% and 69%, respectively. The relative importance of predictor variables in allometric models was dominated by the contribution of REC. Discussion: This work provides an efficient and nondestructive technique to indirectly quantify root biomass of genetically diverse shrub willow progeny, which has great promise for selection of genotypes with varying root biomass and for the accurate estimation of belowground carbon sequestration.

59 BASIC BIOLOGICAL SCIENCES↗

A novel application of cosmic rays for spent nuclear fuel monitoring - 15738

Monitoring nuclear waste and controlling spent nuclear fuel at its source is one of the main strategies to minimize the risks of nuclear proliferation and reduce potential homeland threats. Storage of high level waste from a fission reactor typically involves placing spent fuel in sealed dry casks. After the spent nuclear fuel has been placed inside the dry cask, the cask is welded, not allowing for visual inspection. Conventional methods for examining the interior of materials e.g., X-rays, are limited by the fact that they cannot penetrate very dense well-shielded objects. Instead, cosmic ray muons have the potential to allow for assessment of spent nuclear fuel stored within sealed dense dry casks. Objectives: 1.Exploit the ability of cosmic ray muons to penetrate high density materials allowing the distribution of materials within the object to be inferred from the muon tracks. 2. Develop a monitoring system that tracks the path of cosmic ray muons, including their deflection and attenuation, to identify the contents of a closed dry cask. Methods: - Monte-Carlo simulations using Geant4; - Bayesian decision theory for signal classification; - Wavelet analysis for noise cancellation; - Chaotic Neural Networks for signal encryption. Results: 1. Preliminary statistical analysis proved that the method is feasible and has the ability to identify the presence of spent nuclear fuel in a dry cask. 2. Using monoenergetic muons, a dry cask with one fuel assembly missing can be correctly identified with error rate <1%. Broader merit: Once completed, the proposed project for cosmic ray muon transport will enable a new and potentially transformative approach towards efficient, inexpensive and remote cosmic ray muon applications in archaeology, medicine and safeguarding of nuclear materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Single Crystalline Na 0.67 Ni 0.33 Mn 0.67 O 2 Positive Electrode Material via Molten Salt Synthesis for Sodium Ion Batteries

P2-layered Na 0.67 Ni 0.33 Mn 0.67 O 2 (NNMO) has emerged as a promising positive electrode material for sodium ion batteries due to its appealing electrochemical properties. Synthesis of polycrystalline NNMO (PC-NNMO) materials through conventional calcination of solid precursors remains the prevailing method, where heating occurs in a dry environment with air or O 2 . On the other hand, the molten salt method, where precursors are submerged in molten salt medium during calcination, emerged in recent years to be a scalable technique for more controlled crystal growth and uniform morphology in a variety of materials. Here, we utilize the molten salt method to synthesize single crystalline NNMO (SC-NNMO) materials with enhanced electrochemical properties. The SC-NNMO material exhibits an initial specific discharge capacity of 95 mAh g –1 at a 0.1C rate, retaining approximately 88.5% of its capacity after 100 cycles over a wide voltage range of 2.0–4.2 V. Furthermore, SC-NNMO maintains a capacity retention of 83.9% after 300 cycles at a 1C rate compared to 66.6% for PC-NNMO, indicating excellent long-term cycling stability. This stability is further confirmed by the performance of an SC-NNMO//hard carbon full cell, which retains 90.3% of its capacity after 200 cycles at 1C within a voltage window of 1.9–4.1 V. The enhancement in stability of the SC-NNMO sample is attributed to the single crystalline structure suppressing the undesired P2–O2 phase transition at high voltage. This study also presents an easy, efficient, and straightforward molten salt process for SC-NNMO material synthesis, offering valuable insights into the potential application of such methodology for the large-scale, cost-effective production of various sodium-layered transition metal oxide positive electrode materials for SIBs.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Direct Surface and Droplet Microsampling for Electrospray Ionization Mass Spectrometry Analysis with an Integrated Dual-Probe Microfluidic Chip

Ambient mass spectrometry (MS) has revolutionized the way of MS analysis and broadened its application in various fields. This paper describes the use of microfluidic techniques to simplify the setup and improve the functions of ambient MS by integrating the sampling probe, electrospray emitter probe, and online mixer on a single glass microchip. Two types of sampling probes, including a parallel-channel probe and a U-shaped channel probe, were designed for dryspot and liquid-phase droplet samples, respectively. We demonstrated that the microfabrication techniques not only enhanced the capability of ambient MS methods in analysis of dry-spot samples on various surfaces, but also enabled new applications in the analysis of nanoliter-scale chemical reactions in an array of droplets. The versatility of the microchip-based ambient MS method was demonstrated in multiple different applications including evaluation of residual pesticide on fruit surfaces, sensitive analysis of low-ionizable analytes using postsampling derivatization, and high-throughput screening of Ugi-type multicomponent reactions.

Huang, Cong-Min↗

Partial flocculation for spray drying of spherical mixed metal oxide particles

Abstract Particles are an important design consideration for many proposed solar thermochemical water splitting reactor concepts. These particles must maintain physical integrity and chemical performance at very high temperatures (>900°C) while flowing within a system. Spray drying is a commonly used, scalable method to produce solid spherical particles that have the best opportunity to meet these requirements. Spray drying is used to produce hercynite (FeAl 2 O 4 ) particles using pH ‐modification of a charge‐stabilized sol. This process involves inducing partial flocculation in nanoparticle suspensions to yield larger particles that are spherical and structurally robust. A commercial boehmite suspension is characterized along with a mixture of the boehmite suspension with an iron oxide suspension. Zeta potential near zero and peak yield stress measurements at the same pH indicate flocculation, but associated sedimentation behavior is not observed. The behavior of both the boehmite‐only and mixed suspensions both seem to be driven by the behavior of the boehmite suspension alone. Spray dried particles from the mixed suspension at the critical pH gave significantly larger and more spherical particles, which also indicates flocculation. This relatively simple technique shows promise for new mixed‐metal material formulations and scalable applications.

Ehrhart, Brian D.↗

Laser Cleaning for Decontamination of a Nuclear Facility - 20609

This paper describes laser cleaning of contaminated tools in a nuclear power facility in Chalk River, Ontario Canada and also the same for EnergySolutions facility in Memphis facility. For the Chalk River facility, other methods of cleaning which included dry ice blasting, disassemble and wipe clean and steam cleaning, generated secondary waste and were time consuming. Laser cleaning of the tools in facility did not create secondary waste, was more efficient and safer for the operator. The laser cleaning method was compared with other methods. For the EnergySolutions facility in Memphis, laser cleaning was compared with hands on cleaning and laser removal by applying them to a rail car, a metal plate and a metal skate. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Inspection of Dry Storage Casks Using PGAA and NAA Techniques

In this effort, an assessment of a chloride detection method is performed for inspecting the surfaces of dry cask storage system (DCSS) canisters, with focus on the implementation of a non-destructive nuclear analysis and methodology. Some DCSS canisters (especially those located in coastal environments) will be exposed to marine environments, which can cause atmospheric stress corrosion cracking (SCC). Chloride deposits on canister surfaces provide the corrosive environment necessary for atmospheric SCC with the residual stresses and materials properties conditions. The most susceptible regions on the canister surface are the weld areas, or where cold work has been performed, and may provide the necessary driving force for crack growth. The heat-affected zones (HAZs) near welds are also potentially susceptible to atmospheric SCC due to sensitization of the material caused by chromium depletion during the welding process. Information collected from the field and from laboratory studies has not been able to rule out the possibility of atmospheric chloride induced stress corrosion cracking (CISCC), although no occurrences of atmospheric SCC in DCSS canisters have been detected to-date. A number of researchers have demonstrated that localized corrosion can take place under such situations on materials commonly used for interim storage containers, including 304SS (Cook et al. 2010; Shirai et al. 2011) and 316SS (Tani et al. 2009). In this summary, the preliminary results of a neutron activation analysis (NAA) and prompt gamma activation analysis (PGAA) are performed using MCNP6, a highly sophisticated, multi-particle Monte Carlo simulation code (with the employment of the high performance computing system at the Idaho National Laboratory), and confirm the feasibility of using PGAA and NAA as an environmental inspection methodology for detection and monitoring of small quantities of chlorine on canister surfaces. The specific signature of gamma rays due reactions of sea salt constituents are documented and summarized in this paper. The environmental constituent for passive oxide film breaching is chlorine, which can cause pitting initiation and incubation time that may lead to cracking in stainless steel. Therefore, an assessment of chloride presence at a canister surface is essential before moving to other nondestructive analysis (NDA) methods for detection of pitting and cracking. Two nonlinear acoustic techniques will also be used in our integrated research project (IRP) research study that proves to be useful in the detection of SCC: nonlinear resonant ultrasound spectroscopy (NRUS), and time revisited elastic nonlinear diagnostic (TREND). These two techniques are complementary to marine atmospheric detection techniques. In this presentation only PGAA and NAA are described in detail. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Processing of surrogate nuclear fuel pellets for better dimensional control with dry bag isostatic pressing

A study of improved methods of processing fuel pellets was undertaken using ceria and zirconia/yttria/alumina as surrogates. Through proper granulation and vertical vibration (tapping) of the parts bag prior to dry bag isostatic pressing (DBIP), reproducibility of diameter profiles among multiple pellets of ceria was improved by almost an order of magnitude. Reproducibility of sintered pellets was sufficiently good to possibly avoid grinding. Deviation from the mean diameter along the length of multiple pellets, as well as, deviation from roundness, decreased after sintering. This is not generally observed with dry pressed pellets. Thus it is possible to machine to tolerance before sintering if grinding is necessary.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Performing In Situ Closed-Cell Gas Reactions in the Transmission Electron Microscope

Gas reactions studied by in situ electron microscopy can be used to capture the real-time morphological and microchemical transformations of materials at length scales down to the atomic level. In situ closed-cell gas reaction (CCGR) studies performed using (scanning) transmission electron microscopy (STEM) can separate and identify localized dynamic reactions, which are extremely challenging to capture using other characterization techniques. For these experiments, we used a CCGR holder that utilizes microelectromechanical systems (MEMS)-based heating microchips (hereafter referred to as "E-chips"). The experimental protocol described here details the method for performing in situ gas reactions in dry and wet gases in an aberration-corrected STEM. This method finds relevance in many different materials systems, such as catalysis and high-temperature oxidation of structural materials at atmospheric pressure and in the presence of various gases with or without water vapor. Here, several sample preparation methods are described for various material form factors. During the reaction, mass spectra obtained with a residual gas analyzer (RGA) system with and without water vapor further validates gas exposure conditions during reactions. Integrating an RGA with an in situ CCGR-STEM system can, therefore, provide critical insight to correlate gas composition with the dynamic surface evolution of materials during reactions. In situ/operando studies using this approach allow for detailed investigation of the fundamental reaction mechanisms and kinetics that occur at specific environmental conditions (time, temperature, gas, pressure), in real-time, and at high spatial resolution.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Insights into the Chemistry of the Cathodic Electrolyte Interphase for PTFE-Based Dry-Processed Cathodes

Dry processing is a promising method for high-performance and low-cost lithium-ion battery manufacturing which uses polytetrafluoroethylene (PTFE) as a binder. However, the electrochemical stability of the PTFE binder in the cathodes and the generated chemistry of the cathode electrolyte interphase (CEI) layers are rarely reported. In this work, the CEI properties and PTFE electrochemical stability are studied via cycling the high-loading dry-processed electrodes in electrolytes with LiPF 6 or LiClO 4 salt. Using LiClO 4 salt can eliminate other possible F sources, allowing the decomposition of PTFE to be studied. The detection of LiF in cells with the LiClO 4 salt confirms that PTFE undergoes side reaction(s) in the cathodes. When compared with LiClO 4 , the CEI layer is much thicker when LiPF 6 is used as the electrolyte salt. These results provide insights into the CEI layer and may potentially enlighten the development of binders and electrolytes for the high efficiency and long durability of DP-based LIBs.

25 ENERGY STORAGE↗