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The Qualification of Sealability and Creep Relaxation of Additively Manufactured Zytel Gaskets for PEM Fuel Cells

The purpose of this thesis is to study the feasibility of low-cost additive manufacturing of gaskets for proton exchange membrane fuel cells exposed to extreme temperature conditions ranging from -55°C to 100°C. With the growing popularity and decreasing costs of additive manufacturing technologies, specifically Material Extrusion (ME), research is being conducted to determine the feasibility of ME components. Thermally cycled PEMFCs may exhibit accelerated gasket deterioration, therefore, the mechanical stability of material extruded gaskets following a harsh thermal cycle must be assessed. The feasibility of the material extruded gaskets will be proven by manufacturing optimization and mechanical testing. The target material for this study is Zytel by DuPont Chemical. The mechanical stability will be assessed via sealability and creep relaxation testing according to ASTM F37B and ASTM F38B respectively. Because the capabilities to conduct sealability testing at temperature were not available, each specimen was thermally soaked and allowed to return to room temperature prior to testing. As a result of sealability experiments, the 100°C-soaked specimens resulted in lower leak rates with a higher precision when compared to specimens soaked at -55°C and 22°C at across all compressive loads. It was observed from results from creep relaxation testing that there is thermal contraction and expansion occurring at 55°C and 100°C respectively, which can be observed by the resultant graphs. The recoverability of thermally cycled specimens are better than those that just experienced a high temperature hold. After the seven-day thermal cycle, the samples stabilized and maintained their structure.

Lazarin, Robert↗

Sealability Qualification of Material Extruded Zytel Gaskets at Extreme Temperatures

In this work, an in-depth qualification of additively manufactured Zytel for gasketing proton exchange membrane fuel cells (PEMFC’s) subject to extreme temperature conditions. The temperature cycling of the PEMFC from 55°C to 100°C accelerates the deterioration of these gaskets compared to that of conventional operation. The additive manufacturing process employed to print these gaskets is material extrusion using Zytel filament. In order to see the effects of the temperature of interest on the printed specimen, each specimen was thermally soaked and then charactered and tested according to ASTM standard F37B. ASTM F37B tests a materials ability to seal and maintain it while bearing both a compressive load and internal pressure load to simulate being in static operation. This process of thermally soaking and sealability testing is shown to show the validity of both this material and additive manufactured components for other applications as well. It is observed that soaking the gaskets at 100°C corrects some of the defects that are present after printing such as missing layers and small voids on the surface of the samples. This allowed for the hot soaked materials to perform better than the samples at room temperature and cold soaked.

Sealability↗

Evaluating sealability of blended smart polymer and fiber additive for geothermal drilling with the effect of fracture opening size

Geothermal formations often contain extensive fracture networks. These fracture networks contribute to the significant loss of drilling fluids during geothermal drilling. Multiple loss circulation materials (LCM) such as fiber, granules, and pills have been proposed to tackle this problem but with only limited success. Recent advances in materials science have led to the development of thermoset shape memory polymers (SMP) to address the lost circulation problem. In this paper, we evaluate a thermoset SMP performance in sealing near wellbore fractures of different sizes in geothermal wells. The SMP performance was assessed using granite disks and cylindrical granite cores having fracture sizes of 1000 μm and 3000 μm. A static filtration test was performed using cedar fiber, CaCO 3 , and SMP. Results showed cedar fiber performed better than the CaCO 3 ., reducing fluid loss by 89% and improving sealing pressure by 200 psi. A novel dynamic testing unit that allows for high-temperature testing under flowing conditions was used in this study. The analysis showed that 3% by weight SMP and fiber blends could bridge and plug the 1000 μm fracture. For a larger fracture of 3000 μm width, there was a need to increase the weight concentration of the SMP to 6% to plug the fracture opening effectively. We showed the influence of key parameters such as the type of LCM, concentration, and particle size distribution in optimizing the performance of drilling fluid loss treatment.

02 PETROLEUM↗

Data of High-Temperature Dynamic LCM Testing Setup

Data from high temperature dynamic sealing tests for various fracture widths, at various temperatures (degrees F), with 5 wt.% bentonite-based mud containing various material fiber contents, at 100 to 400 psi differential pressure. Data from pressure test and evaluation of the dynamic lost circulation materials (LCM) testing unit to reflect the condition of open and sealed fracture using fracture width of 1000 microns at 120 degrees F. Links to two papers based on the data - "Loss circulation prevention in geothermal drilling by shape memory polymer" which was published in Geothermics 89 (2021) 101943) as well as "Evaluating sealability of blended smart polymer and fiber additive for geothermal drilling with the effect of fracture opening size", published in the Journal of Petroleum Science and Engineering 206 (2021) 108998.

15 GEOTHERMAL ENERGY↗

Characterization of the mud displacement in an enlarged wellbore: An integrated rock-fluid model

Cement-mud displacement plays a crucial role in the sealability of cement sheaths. Irregular geometric features of a wellbore due to washout can have a negative impact on mud and cement mobilization. An unstable interface between two fluids always leads to mud channeling, interfluid mixing, and cement contamination, degrading the cement quality. Many factors, such as mechanical and rheological properties of fluids, annulus geometry, flow pattern, and flow rate, significantly influence the displacement efficiency. This study investigates the characterization of the mud displacement in an irregular horizontal well using a 3D computational fluid dynamics (CFD) model. Mud is displaced in an enlarged wellbore by geopolymer and neat class G cement. The wellbore geometry is developed based on the caliper log data from an unconventional shale well in the Tuscaloosa Marine Shale (TMS) lithology. The effects of pump rate, density difference, and mud contamination are evaluated by numerical simulations. The results present those residual muds mainly exist in the upper annulus of the enlarged section. Geopolymer has a better sealing performance and can resist more water-based mud (WBM) contaminations than neat class G cement. The scenario with a low mud-cement density difference and high cement injection rate results in a high cement volume fraction, mitigating the gas migration.

58 GEOSCIENCES↗

Property Measurements of the NaCl-PuCl 3 Molten Salt System

Thermal properties of several compositions of the binary NaCl-PuCl 3 salt were measured to confirm the eutectic composition and provide high quality data for use by MSR developers. The PuCl 3 was generated by reducing PuO 2 to plutonium metal in the presence of calcium metal and then chlorinating the metallic plutonium with NH 4 Cl. The resulting PuCl 3 was used to make seven binary NaCl-PuCl 3 compositions with between 59.9 mol % PuCl 3 (Salt 1) and 20.0 mol % PuCl 3 (Salt 7). The eutectic temperature was measured to be 457 ± 4 °C by onset determination in DSC analyses of the seven mixtures, which is consistent with the values in the literature. Additional transitions were observed at approximately 332 and 363 °C in analyses of the PuCl 3 -rich compositions (Salts 1-3) at about 376 and 439 °C in analyses the Na-rich compositions (Salts 4-7). The solid state heat capacity decreased with increasing PuCl 3 content. The liquid state heat capacity was measured for Salt 3 (37.4 mol % PuCl 3 ) and Salt 4 (38.3 mol % PuCl 3 ). A higher heat capacity was measured for Salt 4 and measurements with both salts showed a positive correlation with temperature between 520 and 730 °C. Cells fabricated from nickel and molybdenum for use in DSC measurements at high temperatures could not be adequately sealed because these materials are not sufficiently malleable, even after high temperature annealing. It is recommended that future development focus on corrosion-resistant materials that have mechanical and thermal properties similar to the commercially available gold cells, such as Pt-Rh (80–20) and pure platinum. Those materials are chemically inert, soft, and malleable like gold, but have melting temperatures higher than 1000 °C (Rakhtsaum, 2013). Use of the Pt-Rh alloy should be evaluated first based on superior machinability for making precision parts and its current use in commercial DSC high temperature crucibles. The commercial Pt-Rh cells are not hermetically sealable, but it is expected that cells made from thinner stock can be sealed.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

All-Polyester Multilayer Plastics (‘All-Polyester MLPs’): A Redesign for Inherently Recyclable Plastics

Multilayer plastics (MLPs) are widely used in modern packaging because they combine multiple functions such as oxygen and moisture barriers, mechanical strength, puncture resistance, and heat sealability into lightweight and cost-effective packaging solutions. These attributes are essential for food, beverage, pharmaceutical, and consumer goods packaging. However, conventional commercial MLPs typically consist of five to twelve layers made from chemically incompatible materials, including polyolefins, polyethylene terephthalate, nylon, ethylene-vinyl alcohol (EVOH), adhesives, and tie layers. This complexity makes MLPs extremely difficult to recycle. As a result, the vast majority of multilayer plastics (MLPs) are disposed of through landfilling or incineration. This disposal pathway perpetuates demand for virgin material production, thereby driving high industrial energy consumption, increasing greenhouse gas (GHG) emissions, and contributing to the long-term accumulation of plastic waste. The scope of work included: (1) Design and fabrication of all-polyester multilayer structures using commercially relevant processing methods; (2) Experimental validation of barrier, mechanical, and sealing performance; (3) Demonstration of both mechanical and chemical recycling pathways; and (4) Comprehensive techno-economic analysis (TEA) and life-cycle assessment (LCA) to quantify cost, energy, and environmental impacts.

36 MATERIALS SCIENCE↗