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414 records · Page 23

A Mars Sample Return Sample Handling System

We present a sample handling system, a subsystem of the proposed Dragon landed Mars Sample Return (MSR) mission [1], that can return to Earth orbit a significant mass of frozen Mars samples potentially consisting of: rock cores, subsurface drilled rock and ice cuttings, pebble sized rocks, and soil scoops. The sample collection, storage, retrieval and packaging assumptions and concepts in this study are applicable for the NASA's MPPG MSR mission architecture options [2]. Our study assumes a predecessor rover mission collects samples for return to Earth to address questions on: past life, climate change, water history, age dating, understanding Mars interior evolution [3], and, human safety and in-situ resource utilization. Hence the rover will have "integrated priorities for rock sampling" [3] that cover collection of subaqueous or hydrothermal sediments, low-temperature fluidaltered rocks, unaltered igneous rocks, regolith and atmosphere samples. Samples could include: drilled rock cores, alluvial and fluvial deposits, subsurface ice and soils, clays, sulfates, salts including perchlorates, aeolian deposits, and concretions. Thus samples will have a broad range of bulk densities, and require for Earth based analysis where practical: in-situ characterization, management of degradation such as perchlorate deliquescence and volatile release, and contamination management. We propose to adopt a sample container with a set of cups each with a sample from a specific location. We considered two sample cups sizes: (1) a small cup sized for samples matching those submitted to in-situ characterization instruments, and, (2) a larger cup for 100 mm rock cores [4] and pebble sized rocks, thus providing diverse samples and optimizing the MSR sample mass payload fraction for a given payload volume. We minimize sample degradation by keeping them frozen in the MSR payload sample canister using Peltier chip cooling. The cups are sealed by interference fitted heat activated memory alloy caps [5] if the heating does not affect the sample, or by crimping caps similar to bottle capping. We prefer cap sealing surfaces be external to the cup rim to prevent sample dust inside the cups interfering with sealing, or, contamination of the sample by Teflon seal elements (if adopted). Finally the sample collection rover, or a Fetch rover, selects cups with best choice samples and loads them into a sample tray, before delivering it to the Earth Return Vehicle (ERV) in the MSR Dragon capsule as described in [1] (Fig 1). This ensures best use of the MSR payload mass allowance. A 3 meter long jointed robot arm is extended from the Dragon capsule's crew hatch, retrieves the sample tray and inserts it into the sample canister payload located on the ERV stage. The robot arm has capacity to obtain grab samples in the event of a rover failure. The sample canister has a robot arm capture casting to enable capture by crewed or robot spacecraft when it returns to Earth orbit

Wilson, David↗

Small Fatigue Crack Growth Mechanisms and Interfacial Stability in Cold-Spray 6061 Aluminum Alloys and Coatings

Cold-spray-processed aluminum alloys have static mechanical properties superior to those of aerospace cast alloys, and similar to those of their wrought counterparts, making them good candidates for structural applications. However, their broad and confident use relies upon systematic fatigue crack growth studies to investigate and demonstrate the materials' performance in critical high-integrity components. In this work, the fatigue crack growth behavior in early stages (small crack growth regime) was investigated for cold-spray processed 6061 aluminum alloys and coatings, at stress ratio R = 0.1, in room temperature laboratory air. The effects of the characteristic microstructure and initial flaw size on the fatigue crack growth response were systematically examined, and the crack growth mechanisms at the microstructural scale were established and compared to those of long cracks. The mechanical interfacial stability of coatings was examined in cold-spray 6061-rolled 6061-T6 couples. An original method of quantifying the deposition-substrate interfacial strength, and correlating it to the response under cyclic loading via crack-interface stability maps, was developed. The proposed methodology is based on combined scratch testing and fracture mechanics formulations, and failure at the coating-substrate interface can be predicted for any crack growth scenario under cyclic loading. The method can be broadly used for the design and optimization of cold-spray and other coatings, as well as in structural repair.

36 MATERIALS SCIENCE↗

Elucidating the Role of Carbon Conductive Additive in the Processing and Electrochemical Behavior of Surface-Modified Si Anodes

In the present work, we explore the impact of conducting carbon on the processing of silicon (Si)-rich electrodes, their resulting cycling performance, and parasitic side reactions. We employed three different carbon additives, Super C45 (carbon black), Super C65 (carbon black), and TIMCAL C-NERGY KS 6L (graphite), with varying sizes and morphologies to determine how these parameters influence the structure and the electrochemical behavior of the cast electrodes. Raman mapping indicates that the improved performance achieved using C45 can be explained by the homogeneous distribution of Si and carbon, enabling the formation of continuous electrical pathways throughout the electrode. Further, this finding aligns with the results of ζ potential measurements, which indicate that C45 can maintain more stable dispersions in N-methyl-2-pyrrolidone (NMP) compared with the other carbon additives. However, electrodes with C45 as the conducting agent exhibited increased parasitic side reactions, as evidenced by the leakage current obtained from voltage hold experiments. These side reactions can have adverse effects on the calendar life of the electrode. Furthermore, the Raman maps of the electrodes reveal heterogeneities in Si and carbon distribution with lower carbon content, especially with only 2% carbon. This drastically impacts the cyclability of the electrodes, with portions of the low-carbon electrodes that remain unable to undergo cycling even at slow rates (0.2 Ah g –1 ). Additionally, we found that slower formation rates are favored in the context of parasitic side reactions, although slower formation rates can potentially create thicker passivating films that could hinder Li + -ion transport. Therefore, we emphasize the need for an intricate balance in materials selection and cycling protocol for optimal electrode processing and electrochemical behavior.

25 ENERGY STORAGE↗

Molybdeno-Aluminizing of Powder Metallurgy and Wrought Ti and Ti-6Al-4V alloys by Pack Cementation process

Wear and high temperature oxidation resistance of some titanium-based alloys needs to be enhanced, and this can be effectively accomplished by surface treatment. Molybdenizing is a surface treatment where molybdenum is introduced into the surface of titanium alloys causing the formation of wear-resistant surface layers containing molybdenum, while aluminizing of titanium-based alloys has been reported to improve their high temperature oxidation properties. Whereas pack cementation and other surface modification methods have been used for molybdenizing or aluminizing of wrought and/or cast pure titanium and titanium alloys, such surface treatments have not been reported on titanium alloys produced by powder metallurgy (PM). Also a critical understanding of the process parameters for simultaneous one step molybdeno-aluminizing of titanium alloys by pack cementation and the predominant mechanism for this process have not been reported. The current research work describes the surface modification of titanium and Ti-6Al-4V prepared by PM by molybdeno-aluminizing and analyzes thermodynamic aspects of the deposition process. Similar coatings are also deposited to wrought Ti-6Al-4V and compared. Characterization of the coatings was carried out using scanning electron microscopy and x-ray diffraction. For both titanium and Ti-6Al-4V, the use of a powder pack containing ammonium chloride as activator leads to the deposition of molybdenum and aluminium into the surface but also introduces nitrogen causing the formation of a thin titanium nitride layer. In addition, various titanium aluminides and mixed titanium aluminium nitrides are formed. The appropriate conditions for molybdeno-aluminizing as well as the phases expected to be formed were successfully determined by thermodynamic equilibrium calculations. - Highlights: •Simultaneous co-deposition of Mo-Al onto powder metallurgy and wrought Ti alloy •Thermodynamic calculations were used to optimize deposition conditions •External TiN and internal a Mo-rich layer on all alloy substrates •Titanium aluminides and Ti-Al mixed nitrides are formed on Ti-6Al-4V •The presence of Al and V alloying elements modifies the diffusion of Mo.

36 MATERIALS SCIENCE↗

Solar cell efficiency and high temperature processing of n -type silicon grown by the noncontact crucible method

The capital expense (capex) of conventional crystal growth methods is a barrier to sustainable growth of the photovoltaic industry. It is challenging for innovative techniques to displace conventional growth methods due the low dislocation density and high lifetime required for high efficiency devices. One promising innovation in crystal growth is the noncontact crucible method (NOC-Si), which combines aspects of Czochralski (Cz) and conventional casting. This material has the potential to satisfy the dual requirements, with capex likely between that of Cz (high capex) and multicrystalline silicon (mc-Si, low capex). In this contribution, we observe a strong dependence of solar cell efficiency on ingot height, correlated with the evolution of swirl-like defects, for single crystalline n -type silicon grown by the NOC-Si method. We posit that these defects are similar to those observed in Cz, and we explore the response of NOC-Si to high temperature treatments including phosphorous diffusion gettering (PDG) and Tabula Rasa (TR). The highest lifetimes (2033 us for the top of the ingot and 342 us for the bottom of the ingot) are achieved for TR followed by a PDG process comprising a standard plateau and a low temperature anneal. Further improvements can be gained by tailoring the time-temperature profiles of each process. Lifetime analysis after the PDG process indicates the presence of a getterable impurity in the as-grown material, while analysis after TR points to the presence of oxide precipitates especially at the bottom of the ingot. Uniform lifetime degradation is observed after TR which we assign to a presently unknown defect. Lastly, future work includes additional TR processing to uncover the nature of this defect, microstructural characterization of suspected oxide precipitates, and optimization of the TR process to achieve the dual goals of high lifetime and spatial homogenization.

14 SOLAR ENERGY↗

Influence of microstructure and temperature on impact toughness of H13 steel produced by binder jet additive manufacturing

Binder Jet Additive Manufacturing (BJAM) is a promising manufacturing pathway to produce H13 steel dies and tooling with complex geometries for applications in high pressure aluminum die casting, hot stamping, and injection molding. While fully dense H13 coupons produced using BJAM have been subjected to detailed microstructure characterization, properties which are critical and relevant to the aforementioned applications, such as impact toughness, have not been reported. Here, this work evaluated the influence of microstructural characteristics and test temperature on the impact toughness of H13 produced by BJAM. Coupons were produced from three different powder size distributions (PSDs), with nominal powder size ranges of −22 μm, 10-32 μm, and 15-53 μm. Coupons were printed, sintered, hot isostatically pressed (HIPed), and heat treated by quenching and tempering. After HIPing, the measured porosities of the different PSDs were all less than 0.015 vol%. The −22 μm PSD BJAM material exhibited the best impact toughness of all three PSDs across the entire test temperature range from 25 to 400 °C, and also exhibited an ambient temperature impact toughness of 10.9 J at a hardness of 46 HRC, equivalent to minimum threshold requirements for premium grade H13. However, all three BJAM PSDs exhibited moderately lower impact toughness than premium grade wrought H13 from RT to 400 °C. We attribute this in part due to the very large prior-austenite grain (PAG) sizes near 400 μm and segregation from former liquid channels leading to greater amounts of carbide precipitation on PAG boundaries. Technical pathways for optimizing processing and chemistry of BJAM H13 to further improve impact toughness are discussed.

Binder jet additive manufacturing↗

Affinity and Treatment of LDR Organics in Low Activity Waste by Cementitious Materials – 26109

The physiochemical interactions between organic contaminants, minerals, and polymer additives in grout/cementitious materials are being identified. This research supports a proposed Resource Conservation and Recovery Act (RCRA) treatment variance relevant to the Land Disposal Restriction (LDR) organics present in Hanford tank waste. It provides the technical basis to address the aspects documented by the Environmental Protection Agency in a draft memo necessary to establish that organics can be immobilized/stabilized in a cementitious matrix. The organic species may interact with cementitious minerals, including slag, fly ash, cement, and other components/dopants like activated carbon. A list of 132 reasonably expected LDR organics associated with Hanford tank waste (RPP-RPT-63493, Rev 1a) was screened by functional groups, octanol-water partitioning coefficients, and detection frequency in Hanford tank waste samples. A subset of 15 compounds spanning the identified properties was tested using sorption and leachate tests. These compounds were subjected to traditional batch sorption tests and leaching tests on/from Cast Stone cementitious material with and without activated carbon (a potential organic adsorption additive). The interactions between organic compounds were observed in traditional batch sorption and modified TCLP leachate tests for surrogate Cast Stone material with and without activated carbon addition. Specifically, phthalic acid (negatively charged) and 4-chloroaniline (polar) sorbed strongly to unmodified Cast Stone, while a group of three phenolic compounds (2,4,6-Trichlorophenol, Pentachlorophenol, o-Cresol) sorbed to and were retained by Cast Stone with a 1% activated carbon amendment. Mixtures of these compounds demonstrated visible retention of the organics within the matrix with a quantifiable affinity of the organics to the cement. This novel testing supports the notion that organics within Hanford tank waste would be retained onto the cement phase with the addition of simple materials easily added to the formulation as part of the treatment process. To further provide additional support to this claim, models employing Flory-Huggins theory in conjunction with macromolecular and organic molecule solubility parameters and species activity coefficients are being utilized to better understand these interactions. Within this context, Van Krevelen (VK) and Hansen organic and polymer solubility parameters were used to inform the Flory-Huggins interaction parameter, allowing for a quantifiable method of evaluating polymer-solvent compatibility and, by extension, interactions with proposed binding additives (e.g., activated carbon). These models and measurement should test the hypothesis for our systems understanding and applicability of Flory-Huggins theory, and whether the prediction of organics in the polymer phase versus the aqueous phase can be confidently made using this strategy. The estimation of the organic molecular activity coefficient in these high salt-saturated aqueous systems is another factor that will be assessed. This project aims to predict and understand complicated organic interactions in these heterogenous systems, guiding optimal treatment and stabilization methodologies.

Jolin, Will [Savannah River National Laboratory (S↗

Effective Exploration of New 760°C-Capability Steels for Coal Energy

Cost effective and high performance alloys that are capable of operating at 760 °C or higher for extended periods of time under a very aggressive environment are critically required for the design and development of advanced ultrasupercritical (AUSC) boilers and steam turbines. Finely dispersed Laves phase precipitates have been shown by Takeyama and co-workers to be a viable strengthening mechanism in high temperature austenitic steels. There is currently no straightforward theory that can predict what other intermetallic phases can serve as potent precipitation-strengthening phases for steels; thus we employed a highly effective dual-anneal diffusion multiple (DADM) approach to screen for viable strengthening precipitates over a wide range of compositions. From the Fe-Co-Cr-Ni-Mo DADMs, the Fe-Cr-Mo based Chi phase was identified as a new strengthening phase for high temperature ferritic steels; and from the Fe-Mn-Cr-Nb-Ni-Mo-FeAl DADMs, the Laves phase was identified as a viable strengthening precipitate in Fe-Mn and Fe-Ni based austenitic steels. After identification of viable strengthening phases from the DADMs that covered compositions in the basic ternary and quaternary systems, we employed computation thermodynamics to perform multicomponent alloy design and optimization. For the new the Chi-phase strengthened steels, we performed thermodynamic calculations to vary the volume fraction of the Chi phase and introduced Nb and carbon to promote the formation of stable carbides for grain size control during solution heat treatment. For the Fe-Ni-Mn based austenitic steels, we performed extensive parametric optimization of compositions in order to reduce the expensive Ni content, add Cr and Al for oxidation resistance, and balance the alloying contents (Ni, Mn, Cr, Al, Mo) to suppress the ferritic phase and promote the austenitic matrix phase. Four steels (two ferritic + two austenitic) were designed and tested. The two Chi-phase strengthened ferritic steels exhibited excellent oxidation resistance and good creep-rupture strength at moderate temperatures, considering their ferritic matrix that usually results in lower creep resistance than austenitic steels. These steels showed brittleness and sample-to-sample variability in ductility. The low ductility might be due to the macro segregation during solidification or the significant grain growth during the solution heat treatments. We believe there is no inherent brittleness based on the chemistry of the steels. The creep-rupture performance of the steels is comparable to the 9Cr steels. Due to their ferritic matrix, the new Chi-phase strengthened ferritic steels may not be suited for the 760 °C AUSC applications, but they are very good candidates for intermediate temperature applications due to their outstanding oxidation resistance and high strength. Further study is required to find the source of low and highly variable ductility. We believe the compositions of the Chi-phase strengthened steels are not inherently brittle. The Chi-phase strengthened ferritic steels may also be excellent candidates for intermediate-temperature and room-temperature cast stainless steels, thus we highly recommend further investigations. The two Mn-containing austenitic steels based on the Laves phase showed good ductility, excellent oxidation resistance (slightly inferior to the two ferritic steels) at high temperatures and moderate creep strength. The creep-strength of the two austenitic steels based on the Larson-Miller parameters is higher than that of the traditional 316 stainless steels, but lower than the alumina-forming alloys (AFAs) developed at Oak Ridge National Laboratories. We do not recommend high priority in further studying these compositions unless higher Cr alloys are required for hot-corrosion resistance.

01 COAL, LIGNITE, AND PEAT↗

Integration of Mirror Design with Suspension System using NASA's New Mirror Modeling Software

Advances in mirror fabrication is making very large space based telescopes possible. In the many applications, only monolithic mirrors meet the performance requirements. The existing and near-term planned heavy launch vehicles place a premium on lowest possible mass. Again, available and planned payload shroud size limits near term designs to 4 meter class mirror. Practical 8 meter and beyond designs could encourage planners to include larger shrouds if it can be proven that such mirrors can be manufactured. These two factors lower mass and larger mirrors, presents the classic optimization problem. There is a practical upper limit to how large a mirror can be supported by a purely kinematic mount system and be launched. This paper shows how the design of the suspension system and mirror blank needs to be designed simultaneously. We will also explore the concepts of auxiliary support systems, which act only during launch and disengage on orbit. We will define required characteristics of these systems and show how they can substantially reduce the mirror mass. The AMTD project is developing and maturing the processes for future replacements for HUBBLE, creating the design tools, validating the methods and techniques necessary to manufacture, test and launch extremely large optical missions. This paper will use the AMTD 4 meter "design point" as an illustration of the typical use of the modeler in generating the multiple models of mirror and suspension systems used during the conceptual design phase of most projects. The influence of Hexapod geometry, mirror depth, cell size and construction techniques (Exelsis Deep Core Low Temperature Fusion (c) versus Corning Frit Bonded (c) versus Schott Pocket Milled Zerodur (c) in this particular study) are being evaluated. Due to space and time consideration we will only be able to present snippets of the study in this paper. The advances in manufacturing techniques for lightweight mirrors, such as EXELSIS deep core low temperature fusion, Corning's continued improvements in the Frit bonding process and the ability to cast large complex designs, combined with water-jet and conventional diamond.

Arnold, William↗

Efficient and mechanically-robust organic solar cells based on vertical stratification modulation through sequential blade-coating

Mechanically durable organic solar cells (OSCs) with high efficiency are deemed as the ideal candidate for the power source of the next generation wearable electronic devices. However, the brittle nature of small molecules in most high-efficiency OSCs consisting of polymer and small molecule encourages easy formation of cracks in the photoactive film under deformation. Here, the vertical composition distribution of the active layer has been well optimized through sequential blade coating to realize highly deformable while efficient OSC. The optimized morphology exhibits distinct donor-rich and homogenous region distributed along the vertical direction in the bulk. The donor-rich region provides sufficient chain entanglements and strong interfaces beneficial for mechanical robustness of film, while homogeneously mixed region offers continuous interpenetrating network to maintain high device through-put, resulting in superior efficiency of 14.4% with high crack-onset strain (COS) of 30.5%. This efficiency versus COS combination is much higher than the best combination reported in all polymer systems (COS of 15.9% and efficiency of 11.1%). To the best of our knowledge, it is the highest COS value achieved in polymer-small molecule systems. As a result, the rational control over vertical stratification demonstrated here would guide researchers in the development of innovative wearable electronics.

36 MATERIALS SCIENCE↗

SU-F-T-164: Investigation of PRESAGE Formulation On Signal Quenching in a Proton Beam

Purpose: The radiochromic polyurethane PRESAGE by Heuris Pharma has had limited applications with protons because of a dose response dependence on LET resulting in signal quenching in the Bragg peak. This is due to the radical initiator, a halocarbon, radically recombining in high-LET irradiations. This study investigated the use of alternative halocarbons at various chemical concentrations to determine their significance in signal quenching. Methods: PRESAGE was manufactured in-house and cast in small volume cuvettes (1×1×4cm^3). Several compositions were evaluated to determine the influence of the radical initiator component. Mixtures contained one of two halocarbons, chloroform or bromoform, at concentrations of 5%/10%/15%(w/w). A large volume, cylindrical PRESAGE dosimeter made following the mixture described by Heuris Pharma, 4cm(D)×8.5cm(H), was irradiated with 200-MeV protons to study regions of low- and high-LET along a 10cm spread out Bragg peak isodose profile. Depths corresponding to regions of low quenching (<3%) and high quenching (>20%) were determined. These depths were used for cuvette placement in a solid water phantom. Samples of each formulation were placed at each depth and irradiated to doses between 0 and 10Gy. Results: The cuvettes indicated different levels of quenching for different radical initiator types, concentrations, and total doses. Chloroform formulations showed reduced quenching from 29%(5%-w/w) to 21%(15%-w/w) while bromoform reduced quenching from 27%(5%-w/w) to 17%(15%-w/w). The reduction in quenching was found to be non-linear with concentration of radical initiator. A quenching dose-dependency was also found that changed with formulation. In all cases, quenching was relatively consistent from 0–5Gy but increased at 10Gy. The quenching decreased as concentrations of radical initiator increased. Conclusion: The radical initiator component in PRESAGE is correlated with the signal quenching observed in proton irradiations and formulation adjustments show promise as a method of reducing this quenching. Future work will further investigate concentration limits and optimize the formulation. Grant number 5RO1CA100835.

60 APPLIED LIFE SCIENCES↗

Volumetric Additive Manufacturing of Dormant Catalytic Chemistries to Generate Silicone Micro‐ and Millifluidic Devices and Instant Molds

Tomographic volumetric additive manufacturing (T‐VAM) rapidly prints solid objects within minutes, accessing photochemistries that are traditionally challenging for layer‐based additive manufacturing methods. This includes high‐viscosity materials, air‐free chemistries, and solid‐state systems. Catalytic chemistries are appealing as a pathway to engineering advanced materials, including tough thermosets, silicone elastomers, and complex block copolymers. However, photoactivated dormant catalytic chemistries, where the catalyst irreversibly activates upon exposure to light, are incompatible with typical tomographic VAM approaches. To address this limitation, a zero‐dose optimization strategy is devised to preserve dormant catalysts in desired regions by keeping them unexposed to light. VAM printed micro‐ and millifluidic devices and instant molds are successfully produced within minutes in silicones polymerized using photoactivated dormant platinum photohydrosilylation catalysts. The printed channels are programmed to be 500 and 2500 µm for the micro‐ and millifluidic devices, and print fidelity is assessed by X‐ray computed tomography. This work demonstrates the potential of zero‐dose optimization to expand the range of chemistries accessible for VAM, enabling the rapid fabrication of complex devices.

Additive Manufacturing↗

Physics and the choice of regulators in functional renormalisation group flows

The Renormalisation Group is a versatile tool for the study of many systems where scale-dependent behaviour is important. Its functional formulation can be cast into the form of an exact flow equation for the scale-dependent effective action in the presence of an infrared regularisation. The functional RG flow for the scale-dependent effective action depends explicitly on the choice of regulator, while the physics does not. In this work, we systematically investigate three key aspects of how the regulator choice affects RG flows: (i) We study flow trajectories along closed loops in the space of action functionals varying both, the regulator scale and shape function. Such a flow does not vanish in the presence of truncations. Based on a definition of the length of an RG trajectory, we suggest a constructive procedure for devising optimised regularisation schemes within a truncation. (ii) In systems with various field variables, a choice of relative cutoff scales is required. At the example of relativistic bosonic two-field models, we study the impact of this choice as well as its truncation dependence. We show that a crossover between different universality classes can be induced and conclude that the relative cutoff scale has to be chosen carefully for a reliable description of a physical system. (iii) Non-relativistic continuum models of coupled fermionic and bosonic fields exhibit also dependencies on relative cutoff scales and regulator shapes. At the example of the Fermi polaron problem in three spatial dimensions, we illustrate such dependencies and show how they can be interpreted in physical terms. - Highlights: • We show the regulator dependence of functional renormalisation (FRG) group equations. • Solving FRG equations along closed loops provides a distance between two regulators. • We suggest a practical procedure for devising optimal regulators. • A universality class crossover can be induced by changing relative cutoff scales. • We examine the regulator dependence explicitly in the Fermi polaron problem.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

SU-E-T-353: Effects of Time and Temperature On a Potential Reusable 3D Dosimeter

Purpose: Preliminary studies of a novel, optically-clearing PRESAGE 3D dosimeter formulation (Presage-RU) demonstrated potential reusability. This study investigates the effects of time and temperature on the accuracy and reusability of Presage-RU, and reports on progress toward developing a reusable 3D dosimeter. Methods: Presage-RU was cast as small volume samples (1×1×4.5cm). The effect of dose response sensitivity with reirradiation and time was evaluated by irradiating samples from 0–10Gy, measuring change in optical density (ΔOD), clearing at room temperature (RT) (5–7 days to fully clear), and then repeating for a total of 5 irradiations. Effects of heating on clearing rate were investigated by irradiating samples to 8Gy, then tracking measurements with samples held at RT, 35°C, and 45°C. Two cylindrical dosimeters (11cm diameter, 9.5cm length) were evaluated for dosimetric accuracy when stored at RT and −3°C prior to irradiation. Plans delivered were 2 overlapping AP fields (RT) and VMAT (-3°C). Results: Heating the dosimeters reduced the clearing half-life from 16.3h at RT to 5.8h (35°C) and 5.1h (45°C), but also increased background ΔOD by 1.7x (35°C) and 2.3x (45°C). Reductions in dose response were more closely linked to age than reirradiation, and storage at RT showed pronounced desensitization from dosimeter edges. These results suggest desensitization from oxygen diffusion. It should be noted that atmospheric diffusion into the dosimeter is not seen in standard, single-use PRESAGE, and is likely caused by differences in the Presage-RU polyurethane matrix. The dosimeter kept in cold storage, however, showed no evidence of desensitization and exhibited accuracy on par with standard PRESAGE with a 3%/3mm 3D gamma passing rate of 98.1%. Conclusions: Presage-RU is sensitive to storage temperatures and time, both of which affect oxygen diffusion and subsequent desensitization. Development shows promising progress with further formulation optimization as the next step toward achieving a successful reusable 3D dosimeter. This work was supported by NIH R01CA100835. John Adamovics is the president of Heuris Inc., which commercializes PRESAGE.

60 APPLIED LIFE SCIENCES↗

Gas discharge plasma treatment of poly(ethylene glycol-co-1,3/1,4 cyclohexanedimethanol terephthalate) for enhanced paint adhesion

Low-energy hydrogen-ions and tetrafluoromethane-ions produced from a gas discharge ion source were irradiated to poly(ethylene glycol-co-1,3/1,4 cyclohexanedimethanol terephthalate) (PETG) sheets for enhancing paint adhesion. The ion beams were characterized using a cast steel mass spectrometer, while the untreated and treated samples were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, contact angle measurements, and profilometry. The paint adhesion was determined by using the standard method for evaluating adhesion by knife [ASTM D6677-07, Standard Test Method for Evaluating Adhesion by Knife (ASTM International, West Conshohocken, PA, 2012)] and was correlated with the calculation of the work of adhesion derived from the Young–Dupré equation. After plasma treatment, a significant decrease in the contact angle was observed in all samples, except for the CF{sub 4} ion-treated samples with the discharge current of 3 mA and an irradiation time of 30 min. At longer irradiation times, the treated samples showed lesser changes in the contact angle measurement. The increase in the average and root-mean-square surface roughness was observed on the samples after plasma treatment. The samples treated with either H{sub 2} or CF{sub 4} ions for 15 min showed a direct correlation between the discharge current and surface roughness. The samples treated for 30 min showed no significant correlation between the surface roughness and discharge current, which can be attributed to the possible melting of the samples since PETG has a low melting point. The observation made in this study on the relationship of wettability and surface roughness is consistent with the Wenzel wetting mode. Scanning electron micrographs showed surface etching on the hydrogen ion-treated samples while no significant surface changes were observed for the CF{sub 4} ion-treated samples. In general, paint adhesion was stronger for samples that exhibited enhanced wettability and high work of adhesion. The optimal work of adhesion to double the paint adhesion performance was at least 84.79 mN/m. The increase in the surface roughness after the treatment provided an increased friction between the paint and the PETG surface. The increase in the paint adhesion was also due to the covalent, hydrogen, and van der Waals bonding that are typically observed for highly wettable surfaces.

36 MATERIALS SCIENCE↗

Roll-to-Roll Advanced Materials Manufacturing DOE Laboratory Collaboration - FY2018 Final Report

High-value R2R processing is used to support a wide range of products in applications which span many industrial business sectors. The overall R2R process technology can be considered as “mature” as the process methodology and has been in use for decades. This continuous processing technique traditionally involves deposition of material(s) onto moving webs or carriers or other continuous R2R, belt-fed, or conveyor-based processes that enable successive steps to build a final version which serves to support the deposited materials. Current process technologies, which typify “roll to roll”, include tape casting, silk-screen printing, reel-to-reel vacuum deposition/coating and R2R lithography. Products supported by R2R manufacturing include micro-electronics, electro-chromic window films, PVs, fuel cells for energy conversion, battery electrodes for energy storage, and barrier materials. Due to innovation in materials and process equipment, high-quality yet very low-cost multi-layer technologies can be manufactured on a very cost-competitive basis. To move energy-related products from high-cost niche applications to the commercial sector, a means must be available to enable manufacture of these products in a cost-competitive manner that is affordable by the general consumer. Fortunately, products such as fuel cells, thin- and mid-film PVs, batteries, electrochromic and piezoelectric films, water separation membranes, and other energy saving technologies readily lend themselves to manufacture using R2R approaches.Within the DOE EERE AMO, it was recognized that establishment of a program supported at the DOE National Laboratories, along with their immense design of materials and equipment modelling capabilities enabled with use of high-performance computing, could take advantage of available R2R infrastructure to manufacture new technologies. In FY 2016, a R2R Consortium was established and provided with initial “seed” funding to take an approach that was envisioned to be supportable by advanced manufacturing R2R processes. This collaborative approach was designed to foster identification and development of materials and processes related to R2R for clean-energy product development. Using computational and experimental capabilities by acknowledged subject matter experts within the supported National Laboratory system, this collaborative project would leverage the capabilities and expertise at each of four laboratories to further the development of an enabling high-volume cost-competitive platform technology. The collaboration team that is comprised of ORNL, ANL, NREL and LBNL, coordinating with EPB and other selected industry partners, was formed in April 2016 to initially address enhancing battery electrode performance and R2R manufacturing challenges. The research efforts were to predict and measure changes and results in electrode morphology and performance based on process condition changes; to evaluate mixed, active, particle size deposition and drying for novel electrode materials; to model various process condition changes and the resulting morphology and electrode performance; and to develop and validate NDE techniques for in-line measurement of battery electrode material properties. These efforts carried through FY 2017 and completed at the end of FY 2018.The approach was to look at compositions of materials with different particle sizes to make electrode samples using a R2R manufacturing process. The shape, size, and morphology of the materials, the chemistry of the formulation, the nature of slurries, their coating rate, the rate of drying all play a role in determining the final coating architecture, quality, and performance. A commercial cathode material was selected to make a series of cathodes and anodes by single pass, dual pass and slot die methods. Analysis of all the compiled results for this battery electrode development were that the best performing cathodes included: dual-pass electrode with large particles near the foil, mixed small and large particles, and small particles only. Whereas, the best performing anodes were with a mix of small and large graphite particles. An additional core project was added in FY 2017 to conduct studies of fuel cell materials that can be produced using R2R processes. The goal of this project is to explore, understand and optimize material and process parameters to support increased throughput, increased quality, and reduced cost for high volume production of gas-diffusion electrodes (GDEs) for PEMFCs. Project work in FY 2018 were to use a R2R process to fabricate electrodes without ionomer overlayer that can produce the equivalent mass activity as spray-coated electrodes with an ionomer overlayer. Oxygen-limiting current measurements were utilized to optimize oxygen mass transport. Alcohol-rich solvents were investigated, and results were that the alcohol and water ratio can be tuned to control ionomer distribution. Water-rich solvents produce a more dispersed ink which results in better high-current density performance.

36 MATERIALS SCIENCE↗

NASA's Space Launch System Begins Integration, Stacking in Preparation for Artemis I Launch

The Artemis era of human lunar exploration is nearing take-off as NASA’s new super heavy-lift launch vehicle, the Space Launch System (SLS), begins stack-ing and integration operations in mid-2020 at Kennedy Space Center (KSC) in Florida. With a planned upgrade path to progressively more powerful vehicles and availability in crew and cargo configurations, SLS provides a unique and flexible launch solution to send crew, large-scale infrastructure and robotic probes to deep space. The SLS Block 1 vehicle, the initial variant to fly, is optimized for lunar missions with a proven propulsion system consisting of four liquid hydrogen (LH2)/liquid oxygen (LOX)-fed RS-25 engines and twin five-segment solid rocket boosters (SRBs). The Block 1 vehicle can also be outfitted with an industry-standard 5 m-class payload fairing (the “cargo” configuration) and will launch at least 27 metric tons (t) of mass to trans-lunar injection (TLI). SLS is the backbone of NASA’s Artemis program, which will return the agency’s human spaceflight program to the Moon for the first time since 1972. For the Artemis I mission, SLS will send an uncrewed Orion spacecraft to TLI, where it will enter a distant retrograde lunar orbit and fly 38,000 nmi past the Moon – farther than any spacecraft built for humans has ever traveled. The SLS Block 1 vehicle for Artemis I completed manufacturing in 2019. Several elements, including the upper stage, have been delivered to the Exploration Ground Systems (EGS) program at KSC and are being prepped for integration and stack-ing. The five-segment solid rocket boosters – the largest and most powerful ever built for flight – are also complete. The booster motor segments for the Artemis I flight are scheduled to ship from prime contractor Northrop Grumman’s Utah facilities and begin stacking and integration at KSC in June 2020. The SLS core stage is the largest rocket stage NASA has ever built in terms of volume and height, and includes the avionics and the tanks that feed cryogenic propellant to the four RS-25s (formerly Space Shuttle Main Engines [SSMEs]). They have been modified with an updated controller and nozzle insulation to protect them from the hotter launch environment. The SLS core stage is currently being test-ed at NASA’s Stennis Space Center (SSC) in a series of “green run” tests to verify it meets design and performance requirements. Following the green run test series, which is scheduled to culminate with a full-duration hot-fire of the four RS-25 engines, the core stage will ship to KSC and be stacked between the sol-id rocket boosters in the Vehicle Assembly Building (VAB). Integration of the vehicle will continue with the upper stage, known as the Interim Cryogenic Propulsion Stage (ICPS) and the Launch Vehicle Stage Adapter (LVSA) on the core stage. Another adapter, the Orion Stage Adapter (OSA), connects SLS to Orion and provides housing for 13 6U CubeSat payloads manifested on Artemis I. The CubeSats will be released in deep space after Orion separates from the vehicle, and the flight marks the first ride share opportunity for independent small-sats to deep space. The second major SLS variant to come online, Block 1B, replaces the single-engine ICPS with a four-engine LH2/LOX Exploration Upper Stage (EUS). This more powerful upper stage, along with other vehicle up-grades, will enable the Block 1B vehicle to launch 38-42 t to TLI, depending on crew or cargo configuration. The final evolution of the vehicle, Block 2, will onramp evolved solid rocket boosters to increase mass to TLI to 43-46 t, de-pending on crew or cargo configuration. The Block 1B/Block 2 vehicles can be outfitted with an 8.4 m-diameter payload fairing in 19.1 m or 27.4 m lengths, to provide unprecedented volume for payloads. With the initial Block 1 vehicle completely manufactured and the core stage in final testing before shipping to KSC, the SLS Program and its industry partners have made significant progress manufacturing subsequent vehicles. For the second Block 1 vehicle, the solid rocket motor segments are complete, as are the RS-25 engines with controllers. All five major components of the Artemis II core stage – the forward skirt, LOX and LH2 tanks, intertank and engine section – are manufactured and technicians are installing subsystems at NASA’s rocket factory, Michoud Assembly Facility. The RL-10 engine for the Artemis II ICPS is complete and panels have been machined for its LH2 tank. In addition, panels are machined for the vehicle’s two adapters, with welding scheduled to begin in summer 2020. Flight hard-ware is also in production for the third SLS vehicle, with several booster motor segments cast. The pace of development on the EUS has increased, with the goal to complete Critical Design Review (CDR) in December 2020. Several EUS test rings have been machined at Michoud. The EUS is designed to exe-cute a variety of missions – human spaceflight, deployment of deep-space infra-structure, or high-C3 missions to the outer solar system – with crew and cargo configurations available beginning in the mid-2020s. The near-term goal for the nation’s powerful new space exploration asset, however, is to launch the Arte-mis program, and send the first woman and the next man to the lunar surface. At the Astrodynamics Specialist Conference, the SLS program will update the community on the progress of the initial Block 1 vehicle in final green run test-ing, integration and stacking. In addition, this paper will provide an update to the community on the manufacturing status of subsequent Block 1 and Block 1B vehicles.

Steve Creech↗

Materials for Advanced Ultra-Supercritical (AUSC) Steam Turbines – AUSC Component Demonstration

The work by the United States Department of Energy (U.S. DOE)/Ohio Coal Development Office (OCDO) Advanced Ultra-Supercritical (AUSC) Steam Boiler and Turbine Materials Consortia from 2001 through September 2015 was primarily focused on lab scale and pilot scale materials testing. The field testing included air-cooled probes and steam-cooled “loops” that were installed into existing utility boilers to gain exposure of these materials to realistic conditions of high temperature and corrosion due to the constituents in the coal ash. Successful research and development resulted in identification of metallic alloy materials and fabrication processes suited for power generation applications with metal temperatures up to approximately 1472°F (800°C). These materials or alloys have shown, in extensive laboratory tests and shop fabrication studies, to have excellent applicability for high-efficiency low CO2 transformational power generation technologies. However, as valuable as these material field tests have been for obtaining information, their scale is significantly below that required to minimize the risk associated with a power company building a multi-billion-dollar AUSC power plant. To decrease the identified risk barriers to full-scale implementation of these advanced materials, the U.S. DOE/OCDO AUSC Steam Boiler and Turbine Materials Consortia identified the key areas of the technology that need to be tested at a larger scale. Based upon the recommendations and outcome of a Consortia-sponsored workshop with the U.S.’s leading utilities, a Component Test (ComTest) Program for AUSC was proposed. The AUSC ComTest program would define materials performance requirements, plan for overall advanced system integration, design critical component tests, fabricate components for testing from advanced materials, and carry out the tests. A Pre-FEED evaluation of the test facility including the evaluation of three potential sites has been completed and previously reported. This report describes the Front-End Engineering Design (FEED), Detailed Engineering and the Environmental Assessment of the ComTest project. A significant amount of work was accomplished during Phase 1 to identity the components, as well as the component size, that would be manufactured from advanced alloys such as INCONEL 740H or HAYNES 282 alloys. Pathways to supply these components for ComTest have been identified as well as any further development that would be required. Every project of this nature has challenges and this project was no exception. The greatest challenge has been the project cost. Largely due to the infrastructure and balance of plant equipment upgrades required for Youngstown Thermal, the estimated project cost for the “base case” project was greater than originally budgeted. The project team spent a significant amount of time exploring opportunities for reducing the project cost. These options included: • Youngstown Thermal was exploring building a Combined Heat and Power (CHP) unit at their facility. The Youngstown Thermal staff, supported by Thermal Engineering Group, worked with the project team to determine whether it was economically desirable to supply ComTest with steam and other utilities, which would be supplied by the CHP project. • The project team also evaluated opportunities to optimize the project scope to reduce cost, such as reducing project scope by eliminating the Superheater Outlet Header test. • Southern Company had offered two sites as possible host locations for ComTest. Both sites had infrastructure in place such as steam from an existing unit, natural gas, cooling water and ample electrical power that would be required to be added at the Youngstown Thermal site. Utilizing this existing infrastructure could reduce the project cost. An additional project challenge was the departure of Babcock and Wilcox from the project in September 2016. This project setback was overcome by GE Power’s willingness to assume the design of the ComTest superheater. Since the project could not proceed without the superheater, this was a very positive project development. The merger of the GE Power and Alstom Power steam turbine divisions created synergies leading to the conclusion that instead of building a small-scale turbine, a more practical and useful endeavor would be to validate the manufacturing technology and supplier readiness for fabricating and machining full scale steam turbine components. Consequently, in March 2017, GE Power decided that a steam turbine test would not be necessary as part of the ComTest demonstration. Removing the operational testing of the steam turbine from ComTest further reduced the total project cost. Additionally, there was an opportunity to move ComTest from Youngstown Thermal to one of the Southern Company sites and operate ComTest at supercritical steam conditions and test the steam turbine main stop/control valve at a temperature and pressure that would be representative of the conditions of a high pressure steam turbine inlet valve. The steam could also possibly be returned to the host boiler so there would be no economic penalty of using this steam for ComTest. Relocating the project could further reduce the project cost due to the infrastructure already in place, including high pressure natural gas and cooling water, and the potential for heat integration, allowing a reduction of operating costs. Due to these potential cost reductions, it was decided to move the project away from Youngstown Thermal in March 2017. As integrating ComTest at the Southern Company site was explored, an issue was raised regarding the integration of the ComTest cycle with the plant steam cycle. Steam would be supplied to ComTest at nominally ~3865 psia and 775°F. The steam would be heated with natural gas to 1400°F for the valve test and then cooled to 1000°F so that the steam would be returned to the host boiler at the same conditions as their high pressure steam turbine inlet. However, there were concerns raised that the addition of the energy (natural gas) to the steam could trigger a New Source Review on the unit. Southern Company did not want ComTest to cause this review, so condensing all of the steam exiting ComTest and returning it to the host steam cycle as condensate was explored to insure there would be no implication that ComTest was adding energy to the host plant’s steam cycle. Ultimately, Southern Company decided that they wanted to “decouple” ComTest from the operating unit, making ComTest self-supporting, similar to the Youngstown Thermal “base case.” Without the steam turbine, the project team reached a consensus that operating the ComTest Superheater and steam turbine valves at the typical pressure of a package boiler (~1000 psig) would not generate enough useful technical information to justify the cost of the test. Therefore, it was decided in the December 2017 project quarterly meeting to cancel the operational phase of ComTest. Throughout the engineering phase of ComTest, manufacturing and supply chain challenges were identified. When GE Power recommended dropping the steam turbine test from ComTest, they identified many important manufacturing issues that should be evaluated and demonstrated. Other challenges had been raised by the GE Power group designing the superheater as well as those engineering components such as pressure relief and steam turbine bypass valves. In the December 2017 meeting, the project team decided that it was more beneficial to the AUSC technology to pursue these manufacturing and supply chain issues as Phase 2 of the ComTest project. This report is organized in the following manner: • Section 2 discusses the ComTest project background and organization. • Section 3 discussed project management. • Section 4 discusses the design of the ComTest AUSC components – the Superheater, steam turbine and Superheater Outlet Header. • Section 5 discusses the implementation of ComTest at Youngstown Thermal and the Southern Company site. • Section 6 discusses the development of the AUSC Supply Chain • Section 7 discusses the recommended plan for Phase 2 of ComTest

01 COAL, LIGNITE, AND PEAT↗