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DOE OSTI2012

Developing a Multiscale Test Approach for Characterizing Polymer Composites

A systematic series of experimental characterization efforts have been applied to a novel advanced fiber reinforced nanocomposite material composed of carbon fiber doped with carbon nanotubes in a thermoplastic polymer. A novel depositional process has been developed and refined in order to obtain homogeneous and isotropic dispersion of the CNTs onto the interfacial surface of interest. Fracture mechanics characterization efforts under Mode I and Mode II loading have been investigated to quantify critical strain energy release rate values and study the complex fracture processes. Finite element simulations have complimented the fracture analysis in order to elucidate mechanisms at work during the precipitation and propagation. Thermal analytical responses have been measured using differential scanning calorimetry and thermal gravimetric analysis, while temperature dependent viscoelastic properties have been characterized through variable amplitude dynamic mechanical analysis. Significant increases in the energy absorption characteristics during deformation and fracture behavior have been directly measured for this CNT enhanced material system. This CNT modified CFRP material shows extreme promise for improving interply adhesion and inhibiting delamination.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Sulfur Polymer Stabilization/Solidification Treatability Study of Mercury Contaminated Soil from the Y-12 Site

As a result of past operations, the Department of Energy’s (DOE) Oak Ridge Y-12 National Security Complex (Y-12 Plant) has extensive mercury-contamination in building structures, soils, storm sewer sediments, and stream sediments, which are a source of pollution to the local ecosystem. Because of mercury’s toxicity and potential impacts on human health and the environment, DOE continues to investigate and implement projects to support the remediation of the Y-12 site. URS and #9122;CH2M Oak Ridge LLC (UCOR) under its prime contract with DOE has cleanup responsibilities on the DOE Oak Ridge Reservation and is investigating potential mercury-contaminated soil treatment technologies through an agreement with Babcock and Wilcox (B and W) Y-12, the Y-12 operating contractor to DOE. As part of its investigations, UCOR has subcontracted with Brookhaven National Laboratory (BNL) to conduct laboratory-scale studies evaluating the applicability of the Sulfur Polymer Stabilization/Solidification (SPSS) process using surrogate and actual mixed waste Y-12 soils containing mercury (Hg) at 135, 2,000, and 10,000 ppm. SPSS uses a thermoplastic sulfur binder to convert Hg to stable mercury sulfide (HgS) and solidifies the chemically stable product in a monolithic solid final waste form to reduce dispersion and permeability. Formulations containing 40 – 60 dry wt% Y-12 soil were fabricated and samples were prepared in triplicate for Environmental Protection Agency Toxicity Characteristic Leaching Procedure (TCLP) testing by an independent laboratory. Those containing 50 and 60 wt% soil easily met the study criteria for maximum allowable Hg concentrations (47 and 1 ppb, respectively compared with the TCLP limit of 200 ppb Hg). The lowest waste loading of 40 wt% yielded TCLP Hg concentrations slightly higher (240 ppb) than the allowable limit. Since the Y-12 soil tended to form clumps, the improved leaching at higher waste loadings was probably due to reduction in particle size from friction of the soil mixing, which creates more surface area for chemical conversion. This was corroborated by the fact that the same waste loading pre-treated by ball milling to reduce particle size prior to SPSS processing yielded TCLP concentrations almost 30 times lower, and at 8.5 ppb Hg was well below EPA limits. Pre-treatment by ball milling also allowed a reduction in the time required for stabilization, thus potentially reducing total process times by 30%.Additional performance testing was conducted including measurement of compressive strength to confirm mechanical integrity and immersion testing to determine the potential impacts of storage or disposal under saturated conditions. For both surrogate and actual Y-12 treated soils, waste form compressive strengths ranged between 2,300 and 6,500 psi, indicating very strong mechanical integrity (a minimum of greater than 40 times greater than the NRC guidance for low-level radioactive waste). In general, compressive strength increases with waste loading as the soil acts as an aggregate in the sulfur concrete waste forms. No statistically significant loss in strength was recorded for the 30 and 40 wt% surrogate waste samples and only a minor reduction in strength was measured for the 43 wt% waste forms. The 30 wt% Y-12 soil did not show a significant loss in strength but the 50 wt% samples were severely degraded in immersion due to swelling of the clay soil. The impact on Hg leaching, if any, was not determined.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2013

Miscibility Evaluation Of The Next Generation Solvent With Polymers Currently Used At DWPF, MCU, And Saltstone

The Office of Waste Processing, within the Office of Technology Innovation and Development, funded the development of an enhanced Caustic-Side Solvent Extraction (CSSX) solvent for deployment at the Savannah River Site for removal of cesium from High Level Waste. This effort lead to the development of the Next Generation Solvent (NGS) with Tris (3,7-dimethyl octyl) guanidine (TiDG). The first deployment target for the NGS solvent is within the Modular CSSX Unit (MCU). Deployment of a new chemical within an existing facility requires verification that the new chemical components are compatible with the installed equipment. In the instance of a new organic solvent, the primary focus is on compatibility of the solvent with organic polymers used in the affected facility. This report provides the calculated data from exposing these polymers to the Next Generation Solvent. An assessment of the dimensional stability of polymers known to be used or present in the MCU, Defense Waste Processing Facility (DWPF), and Saltstone facilities that will be exposed to the NGS showed that TiDG could selectively affect the elastomers and some thermoplastics to varying extents, but the typical use of these polymers in a confined geometry will likely prevent the NGS from impacting component performance. The polymers identified as of primary concern include Grafoil ® (flexible graphite), Tefzel ® , Isolast ® , ethylene-propylene-diene monomer (EPDM) rubber, nitrile-butadiene rubber (NBR), styrene-butadiene rubber (SBR), ultra high molecular weight polyethylene (UHMWPE), and fluorocarbon rubber (FKM). Certain polymers like NBR and EPDM were found to interact mildly with NGS but their calculated swelling and the confined geometry will impede interaction with NGS. In addition, it was found that Vellumoid (cellulose fibers-reinforced glycerin and protein) may leach protein and Polyvinyl Chloride (PVC) may leach plasticizer (such as Bis-Ethylhexyl-Phthalates) into the NGS solvent. Either case will not impact decontamination or immobilization operations at Savannah River Site (SRS). Some applications have zero tolerance for dimensional changes such as the operation of valves while other applications a finite dimensional change improves the function of the application such as seals and gaskets. Additional considerations are required before using the conclusions from this work to judge outcomes in field applications. Decane, a component of Isopar L that is most likely to interact with the polymers, mildly interacted with the elastomers and the propylene based polymers but their degree of swelling is at most 10% and the confined geometry that they are typically placed in indicate this is not significant. In addition, it was found that Vellumoid may leach protein into the NGS solvent. Since Vellumoid is used at the mixer in Saltstone where it sees minimum quantities of solvent, this leaching has no effect on the extraction process at MCU or the immobilization process at saltstone. No significant interaction is expected between MaxCalix and the polymers and elastomers used at MCU, DWPF, and Saltstone. Overall, minimal and insignificant interactions are expected on extraction and immobilization operations when MCU switches from CSSX to NGS solvent. It is expected that contacting NGS will not accelerate the aging rate of polymers and elastomers under radiation and heat. This is due to the minimal interaction between NGS and the polymers and the confined geometries for these polymers. SRNL recommends the use of the HSP method (for screening) and some testing to evaluate the impact of other organic such as alcohols, glycolate, and their byproducts on the polymers used throughout the site.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Reduced Parasitic Lasing in Ti:Sapphire Lasers. Removing a Bottleneck to New Ways of Acceleration

Powerful solid state lasers can be efficient sources of high energy electrons in a new concept of particle acceleration. One limitation to the power of these lasers is the phenomenon of parasitic lasing, in which oscillations transverse to the intended lasing direction can drain the stored energy and thus clamp the gain at some maximum value. This problem becomes more severe the larger the laser crystal becomes. The source of the problem is the internal reflections in the larger sized gain material. This program was aimed at eliminating this bottleneck to more powerful lasers, to allow more intense high energy beams to be generated by this technique. The basic approach was to eliminate the internal reflections by making an absorbing layer on the outside of the crystal that had the same refractive index as the crystal. Thus, any transverse light would be absorbed before it reached the edge of the crystal and had a chance to reflect back into the interior. During the first year, furnaces were renovated that and used to produce evaluation crystals. The first approach was to oxidize the outside surface of the titanium doped sapphire laser gain crystal. This oxidation is known to make the crystal be absorbing in the lasing wavelengths. A number of tests showed some modest absorption. After the first year, 2 parallel paths were pursued to improve on this initial results – overgrowth and oxidation and grooving with index matched thermoplastic. Experiments on one of these techniques progressed to near-operational status as a commercial coating process. A test Ti:sapphire rod with a commercial coating technique was also supplied to the subcontractor for baseline testing. The final product of the Phase II was a process that was reduced to a commercialized operation involving the complex series of steps of fabricating the crystal, polishing, grooving, providing an AR coating, then producing the absorbing layer and packaging the crystal in a manner that would allow easy handling for installation and deinstallation.

43 PARTICLE ACCELERATORS↗

DOE OSTI2015

Evaluation of advanced polymers for additive manufacturing

The goal of this Manufacturing Demonstration Facility (MDF) technical collaboration project between Oak Ridge National Laboratory (ORNL) and PPG Industries, Inc. was to evaluate the feasibility of using conventional coatings chemistry and technology to build up material layer-by-layer. The PPG-ORNL study successfully demonstrated that polymeric coatings formulations may overcome many limitations of common thermoplastics used in additive manufacturing (AM), allow lightweight nozzle design for material deposition and increase build rate. The materials effort focused on layer-by-layer deposition of coatings with each layer fusing together. The combination of materials and deposition results in an additively manufactured build that has sufficient mechanical properties to bear the load of additional layers, yet is capable of bonding across the z-layers to improve build direction strength. The formulation properties were tuned to enable a novel, high-throughput deposition method that is highly scalable, compatible with high loading of reinforcing fillers, and is inherently low-cost.

36 MATERIALS SCIENCE↗

DOE OSTI2016

State-of-the-art in Manufacturing Pyrochemical Processing Crucibles

Engineers at Los Alamos National Laboratory have been purifying plutonium through pyrochemical processing for many years. The harsh environments involved with the pyrochemical processes include high temperatures (700-900 °C), molten salts and reactive metals (MgCl 2 , PuCl 3 , NaCl-KCl, CaCl 2 , Pu, Ca), and chlorine gas. Because of these corrosive conditions, designing and developing the pyrochemical processing equipment has always been an intriguing technical challenge. In this article I focus on the design and development of the pyrochemical processing crucible for the electrorefining (ER) process, applying design for manufacturability principles throughout the process. I review the current crucible design and electrorefining process and explore possibilities of making the crucible as one part, building the anode and cathode into the crucible, and various material of construction improvements. Materials of construction that should be reviewed further include alumina, silicon nitride, and a tantalum carbon alloy. I briefly review the application of three-dimensional (3D) printing to the process of producing the ER crucible, including thermoplastic 3D printing and mechanical property concerns. I finish by summarizing current plans and possibilities of improving the ER crucible.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

A Literature Review on the Study of Moisture in Polymers

This literature review covers the main chemical and physical interactions between moisture and the polymer matrix. Fickian versus Non-Fickian diffusion behaviors are discussed in approximating the characteristics of moisture sorption. Also, bound water and free water sorbed in polymers are distinguished. Methods to distinguish between bound and free water include differential scanning calorimetry, infrared spectroscopy, and time-domain nuclear magnetic resonance spectroscopy. The difference between moisture sorption and water sorption is considered, as well as the difficulties associated with preventing moisture sorption. Furthermore, specific examples of how moisture sorption influences polymers include natural fiber-polymer composites, starch-based biodegradable thermoplastics, and thermoset polyurethane and epoxies.

36 MATERIALS SCIENCE↗

DOE OSTI2016

CRADA/NFE-15-05761 Report: Additive Manufacturing of Isotropic NdFeB Bonded Permanent Magnets

The technical objective of this technical collaboration phase I proposal is to fabricate net shape isotropic NdFeB bonded magnets utilizing additive manufacturing technologies at the ORNL MDF. The goal is to form complex shapes of thermoplastic and/or thermoset bonded magnets without expensive tooling and with minimal wasted material. Two additive manufacturing methods; the binder jet process; and big area additive manufacturing (BAAM) were used. Binder jetting produced magnets with the measured density of the magnet of 3.47 g/cm 3 , close to 46% relative to the NdFeB single crystal density of 7.6 g/cm 3 were demonstrated. Magnetic measurements indicate that there is no degradation in the magnetic properties. In addition, BAAM was used to fabricate isotropic near-net-shape NdFeB bonded magnets with magnetic and mechanical properties comparable or better than those of traditional injection molded magnets. The starting polymer magnet composite pellets consist of 65 vol% isotropic NdFeB powder and 35 vol% polyamide (Nylon-12). The density of the final BAAM magnet product reached 4.8 g/cm 3 , and the room temperature magnetic properties are: Intrinsic coercivity Hci = 8.65 kOe, Remanence Br = 5.07 kG, and energy product (BH) max = 5.47 MGOe (43.50 kJ/m 3 ). This study provides a new pathway for preparing near-net shape bonded magnets for various magnetic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Instrumentation Cables Test Plan

A fire at a nuclear power plant (NPP) has the potential to damage structures, systems, and components important to safety, if not promptly detected and suppressed. At Browns Ferry Nuclear Power Plant on March 22, 1975, a fire in the reactor building damaged electrical power and control systems. Damage to instrumentation cables impeded the function of both normal and standby reactor coolant systems, and degraded the operators’ plant monitoring capability. This event resulted in additional NRC involvement with utilities to ensure that NPPs are properly protected from fire as intended by the NRC principle design criteria (i.e., general design criteria 3, Fire Protection). Current guidance and methods for both deterministic and performance based approaches typically make conservative (bounding) assumptions regarding the fire-induced failure modes of instrumentation cables and those failure modes effects on component and system response. Numerous fire testing programs have been conducted in the past to evaluate the failure modes and effects of electrical cables exposed to severe thermal conditions. However, that testing has primarily focused on control circuits with only a limited number of tests performed on instrumentation circuits. In 2001, the Nuclear Energy Institute (NEI) and the Electric Power Research Institute (EPRI) conducted a series of cable fire tests designed to address specific aspects of the cable failure and circuit fault issues of concern1. The NRC was invited to observe and participate in that program. The NRC sponsored Sandia National Laboratories to support this participation, whom among other things, added a 4-20 mA instrumentation circuit and instrumentation cabling to six of the tests. Although limited, one insight drawn from those instrumentation circuits tests was that the failure characteristics appeared to depend on the cable insulation material. The results showed that for thermoset insulated cables, the instrument reading tended to drift and fluctuate, while the thermoplastic insulated cables, the instrument reading fell off-scale rapidly. From an operational point of view, the latter failure characteristics would likely be identified as a failure from the effects of fire, while the former may result in inaccurate readings.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2017

Summer 2017 Microfluidics Research Report

Liquid-liquid Extraction (LLE), also known as solvent extraction, represents a large subset of chemistry where one or more solutes are transferred across an interface between two immiscible liquids. This type of chemistry is used in industrial scale processes to purify solvents, refine ore, process petroleum, treat wastewater, and much more. Although LLE has been successfully employed at the macroscale, where many liters/kgs of species are processed at large flow rates, LLE stands to benefit from lab-on-a-chip technology, where reactions take place quickly and efficiently at the microscale. A device, called a screen contactor, has been invented at Los Alamos National Laboratory (LANL) to perform solvent extraction at the microscale. This invention has been submitted to LANL’s Feynman Center for Innovation, and has been filed for provisional patent under U.S. Patent Application No. 62/483,107 1. The screen contactor consists of a housing that contains two different screen materials, flametreated stainless steel and polyether ether ketone (PEEK) thermoplastic, that are uniquely wetted by either an aqueous or an organic liquid phase, respectively. Liquids in this device flow longitudinally through the screens. The fine pore size of the screens (tens of microns) provide large capillary/adhesional forces while maintaining small hydraulic pressure drops. These physical characteristics are paramount to efficient microscale liquid phase separation. To demonstrate mass transfer using the screen contactor, a well-known chemical system 2 consisting of water and n-decane as solvents and trimethylamine (TEA) as a solute was selected. TEA is basic in water so its concentration can easily be quantified using a digital pH meter and an experimentally determined base dissociation constant. Characterization of this solvent system and its behavior in the screen contactor have been the focus of my research activities this summer. In the following sections, I have detailed experimental results that have been gathered.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Validation of Material Models For Automotive Carbon Fiber Composite Structures Via Physical And Crash Testing (VMM Composites Project)

As automotive fuel economy requirements increase, the push for reducing overall vehicle weight will likely include the consideration of materials that have not previously been part of mainstream vehicle design and manufacturing, including carbon fiber composites. Vehicle manufacturers currently rely on computer-aided engineering (CAE) methods as part of the design and development process, so going forward, the ability to accurately and predictably model carbon fiber composites will be necessary. If composites are to be used for structural components, this need applies to both, crash and quasi-static modeling. This final report covers the results of a five-year, $6.89M, 50% cost-shared research project between Department of Energy (DOE) and the US Advanced Materials Partnership (USAMP) under Cooperative Agreement DE-EE-0005661 known as “Validation of Material Models for Automotive Carbon Fiber Composite Structures Via Physical and Crash Testing (VMM).” The objective of the VMM Composites Project was to validate and assess the ability of physics-based material models to predict crash performance of automotive primary load-carrying carbon fiber composite structures. Simulation material models that were evaluated included micro-mechanics based meso-scale models developed by the University of Michigan (UM) and micro-plane models by Northwestern University (NWU) under previous collaborations with the DOE and Automotive Composites Consortium/USAMP, as well as five commercial crash codes: LS-DYNA, RADIOSS, VPS/PAM-CRASH, Abaqus, and GENOA-MCQ. CAE predictions obtained from seven organizations were compared with experimental results from quasi-static testing and dynamic crash testing of a thermoset carbon fiber composite front-bumper and crush-can (FBCC) system gathered under multiple loading conditions. This FBCC design was developed to demonstrate progressive crush, virtual simulation, tooling, fabrication, assembly, non-destructive evaluation and crash testing advances in order to assess the correlation of the predicted results to the physical tests. The FBCC was developed to meet a goal of 30-35% mass reduction while aiming for equivalent energy absorption as a steel component for which baseline experimental results were obtained from testing in the same crash modes. The project also evaluated crash performance of thermoplastic composite structures fabricated from commercial prepreg materials and low cost carbon fiber sourced from Oak Ridge National Laboratory. The VMM Project determined that no set of predictions from a CAE supplier were found to be universally accurate among all the six crash modes evaluated. In general, crash modes that were most dependent on the properties of the prepreg were more accurate than those that were dependent on the behavior of the joints. The project found that current CAE modeling methods or best practices for carbon fiber composites have not achieved standardization, and accuracy of CAE is highly reliant on the experience of its users. Coupon tests alone are not sufficient to develop an accurate material model, but it is necessary to bridge the gap between the coupon data and performance of the actual structure with a series of subcomponent level tests. Much of the unreliability of the predictions can be attributed to shortcomings in our ability to mathematically link the effects of manufacturing and material variability into the material models. This is a subject of ongoing research in the industry. The final report is organized by key technical tasks to describe how the validation project developed, modeled and compared crash data obtained on the composite FBCC to the multiple sets of CAE predictions. Highlights of the report include a discussion of the quantitative comparison between predictions and experimental data, as well as an in-depth discussion of remaining technological gaps that exist in the industry, which are intended to spur innovations and improvements in CAE technology.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Response of Nuclear Power Plant Instrumentation Cables Exposed to Fire Conditions.

This report presents the results of instrumentation cable tests sponsored by the US Nuclear Regulatory Commission (NRC) Office of Nuclear Regulatory Research and performed at Sandia National Laboratories (SNL). The goal of the tests was to assess thermal and electrical response behavior under fire-exposure conditions for instrumentation cables and circuits. The test objective was to assess how severe radiant heating conditions surrounding an instrumentation cable affect current or voltage signals in an instrumentation circuit. A total of thirty-nine small-scale tests were conducted. Ten different instrumentation cables were tested, ranging from one conductor to eight-twisted pairs. Because the focus of the tests was thermoset (TS) cables, only two of the ten cables had thermoplastic (TP) insulation and jacket material and the remaining eight cables were one of three different TS insulation and jacket material. Two instrumentation cables from previous cable fire testing were included, one TS and one TP. Three test circuits were used to simulate instrumentation circuits present in nuclear power plants: a 4–20 mA current loop, a 10–50 mA current loop and a 1–5 VDC voltage loop. A regression analysis was conducted to determine key variables affecting signal leakage time.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2017

Biobased bamboo composite development

Resource Fiber LLC identified that bamboo fiber could be integrated with synthetic materials to create stronger, lighter weight and “greener” products. In this Phase I work, Resource Fiber collaborated with the Manufacturing Demonstration Facility of Oak Ridge National Laboratory and the University of Tennessee (MDF). The goal of the collaboration was to conduct proof of concept studies on bamboo fibers with thermoset and thermoplastic resins with a view to create commercial products.

09 BIOMASS FUELS↗

DOE OSTI2017

Evaluation of Advanced Polymers for Additive Manufacturing

The goal of this Manufacturing Demonstration Facility (MDF) technical collaboration project between Oak Ridge National Laboratory (ORNL) and PPG Industries, Inc. (PPG) was to evaluate the feasibility of using conventional coatings chemistry and technology to build up material layer-by-layer. The PPG-ORNL study successfully demonstrated that polymeric coatings formulations may overcome many limitations of common thermoplastics used in additive manufacturing (AM), allow lightweight nozzle design for material deposition, and increase build rate. The materials effort focused on layer-by-layer deposition of coatings with each layer fusing together. The combination of materials and deposition results in an additively manufactured build that has sufficient mechanical properties to bear the load of additional layers, yet is capable of bonding across the z-layers to improve build direction strength. The formulation properties were tuned to enable a novel, high-throughput deposition method that is highly scalable, compatible with high loading of reinforcing fillers, and inherently low-cost.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Additive Manufacturing for Highly Efficient Window Inserts

ORNL partnered with the Mackinac Technology Company to demonstrate how additive manufacturing can be used to create highly energy efficient window inserts for retrofit in pre-existing buildings. Many early iterations of the window inserts were fabricated using carbon fiber reinforced thermoplastics and polycarbonate films as a stand in for the low-e coated films produced by the Mackinac Technology Company. After demonstration of the proof of concept, i.e. custom window inserts with tensioned film, the materials used for the manufacture of the frames was more closely examined. Hollow particle-filled syntactic foam and low-density polymer composites formed by expandable microspheres were explored as the materials used to additively manufacture the frames of the inserts. It was concluded that low-cost retrofit window inserts in custom sizes could be easily fabricated using large scale additive manufacturing. Furthermore, the syntactic and expanded foams developed and tested satisfy the mechanical performance requirements for the application.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Conformable Hydrogen Storage Pressure Vessel

Existing commercially available hydrogen storage technologies are largely based on bulky and costly pressure vessels. These pressure vessels come in various forms, ranging from Type I steel cylinders to Type III and Type IV composite wrapped cylinders with metallic or polymer liners. In efforts to increase the pressure vessel storage density and meet DOE hydrogen storage targets, manufacturers are making incremental improvements. This approach alone is unlikely to meet DOE hydrogen storage targets and increase adoption of hydrogen fuel cell vehicles. The project team, led by the Center for Transportation and the Environment (CTE) and consisting of High Energy Coil Reservoirs, LLC (HECR) and The University of Texas at Austin's Center for Electromechanics (UT-CEM), has investigated a transformational hydrogen storage technology using high pressure modulus polymeric pressure vessels. These vessels are constructed by overwrapping an extruded thermoplastic elastomeric resin liner with high performance tensile fiber. This technology is used in commercially available compressed air storage for firefighters. The result is a lightweight, flexible, non-explosive, and non-fragmenting pressure vessel that can be shaped (prior to pressurization) to conform to specific applications. Although this project was funded to investigate the potential for this technology for vehicle applications, a potential significant cost reduction allowed with this approach may make it effective for high pressure ground storage as well. As part of Phase I of this project, the research team demonstrated a Kevlar™ over-braid that achieves a burst pressure in excess of 3.1X the operating pressure of 700 bar. The conformable vessel is able to achieve this pressure rating with reduced weight and cost when compared to Type IV vessels. The researchers also identified two potential resins to serve as the liner of the vessel. These resins have excellent hydrogen barrier properties that could enable a liner thickness of 0.06 inches or less; however, difficulties in manufacturing the core due to the extrusion manufacturing processes required testing with prototype resins as commercially available resins were not found that had the required properties. The team was able to build and test a vessel with one such blend, which outperformed the baseline Hytrel resin materials but did not meet the project hydrogen permeability rate goals.

08 HYDROGEN↗

DOE OSTI2014

Response Bias of Electrical Cable Coatings at FIRE Conditions (REBECCA-FIRE)

This report presents the results of a series of cable fire-retardant coating tests sponsored by the US Nuclear Regulatory Commission (NRC) Office of Nuclear Regulatory Research and performed at Sandia National Laboratories in conjunction with the National Institute of Standards and Technology (NIST). The goal of the tests was to assess the effects of three commercially available fire-retardant cable coating materials on cable thermal and electrical response behavior under fire-exposure conditions. The specific test objectives were to assess, under severe radiant heating conditions, how the coating materials impacted (1) cable thermal response and (2) electrical integrity behavior. The tests were not explicitly designed to assess the impact of the coatings on cable flammability, although some insights relative to the burning behavior of the coating materials themselves and cable ignition times were gained. NIST is currently investigating these attributes under the Cable Heat Release, Ignition, and Spread in Tray Installations During Fire (CHRISTIEFIRE) program (NUREG/CR-7010). The cables used in construction of the test articles were all seven-conductor 12AWG (American wire gage) control or power type copper conductor electrical cables. Two cable insulation types were represented, a polyethylene thermoplastic material and a cross-linked polyethylene thermoset material. Both cable types used have been tested extensively in recent NRC-sponsored experimental programs involving both circuit failure modes and effects testing and fire growth testing. The test articles included uncoated cables and cables coated with one of three fire-retardant coating materials: Carboline Intumastic 285, Flamemastic F-77, and Vimasco 3i. Test configurations included single lengths of cables, bundles of seven cables, and bundles of ten cables. The tests show that, under certain conditions, the fire-retardant coatings provide a substantial benefit relative to delays in cable heating, ignition and electrical failure times. However, as has been seen in prior test programs, the performance varied substantially among the coating products. The current tests also show that the benefit gained by the coatings was heavily dependent on the thermal mass of the coated cable system. Low thermal mass systems, such as the single lengths of coated cable, saw essentially no net benefit from application of the coatings. Intermediate mass systems, represented by the seven-cable bundles, saw some benefit from application of the coatings, but the benefit was inconsistent, and some cables in the bundles saw essentially no delay in thermal response or time to failure. For the larger thermal mass systems, represented by the ten-cable bundles, the benefit of the coatings was both more pronounced and more consistent with all coatings providing a measurable benefit.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Design and Characterization of High Thermal Conductivity Pipes from Roll-to- Roll Processed Hybrid Copper-Polymer Strips for Waste Heat Recovery

Metal based heat exchangers targeting low temperature (<150°C) waste heat recovery (WHR) face high maintenance and material costs [1] that result in long payback periods (>1 year). Low-cost polymer pipes suffer from poor thermal conductivity (~0.2 W/m.K), and thus a low overall heat transfer coefficient. Previous reports demonstrated thermal conductivity enhancement in polymers through systematic molecular alignment [2, 3, 4], or by metal micro-particle inclusions [5]. However, these approaches suffer from scalability issues for WHR heat exchangers in terms of cost [1, 3], and thermomechanical considerations [6, 7]. In this work, we propose hybrid metal-polymer strips that are strategically designed to enhance thermal conductivity by cladding copper around polymer strips. The polymer strips with copper-clad edges are wound helically to form the pipes for a heat exchanger. Through numerical simulations, we optimize the copper-polymer strip layouts to achieve high wall thermal conductivity (k > 1 W/m.K) and also have low volume fraction of copper (<70%) for the composite pipes. In copper-polymer composite heat exchangers, the bottlenecks for heat transfer are the thermal interfacial resistances of copper-copper and copper-polymer joints. We experimentally measured interfacial resistances to be ~1x10 -5 K.m 2 /W and ~4x10 -5 K.m 2 /W for copper-copper and copper-polymer joints, respectively. Using the measured interfacial resistances, we further optimized the design of the hybrid pipes to find high thermal conductivity (> 1 W/m.K) designs. We predict up to ~20 % enhancement in overall heat transfer relative to an all polymer (k = 0.2 W/m.K) heat exchanger system. Using a cohesive zone modelling (CZM) for predicting delamination at the weld joints, we find that our hybrid pipes can have operating internal pressures > 200 psi. The optimized designs of hybrid metal-polymer pipes provide a scalable and cost- effective means for harvesting waste heat from low temperature sources. Thekdi, A., and Nimbalkar, S. Oak Ridge National Lab (2014). Shen, Sheng, et al. Nature nanotechnology 5.4 (2010). Xu, Yanfei, et al. Science advances 4.3 (2018). Smith et al. ACS nano, 9(2), (2015). Sofian, N.M., et al., Journal of Thermoplastic Composite Materials (2001). Aymonier et al. Chemistry of Materials, 15(25), (2003). Tavman, I.H., Journal of Applied Polymer Science, 62(12), (1996).

C Rajagopal, Manjunath↗