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At least 937 records · Page 52

Core Characterization of Bakken Shale from the Bedwell 33-52-1-1H Well, Sheridan County, Montana

The computed tomography (CT) facilities and the Multi-Sensor Core Logger (MSCL) at the National Energy Technology Laboratory (NETL) in Morgantown, West Virginia were used to characterize core of the Bedwell 33-52-1-1H well (API 25-091-21920), a wildcat field in Sheridan County, Montana. The primary impetus of this work is to provide a unique dataset to researchers at universities, national laboratories, geological surveys, and other locations for additional analyses. The resultant datasets are presented in this report and can be accessed from NETL's Energy Data eXchange (EDX) online system using the following link: https://edx.netl.doe.gov/dataset/bedwell-33-52-1-1h-well. The equipment and techniques used to characterize the full core were non-destructive, enabling future examinations and analyses to be performed on these cores. However, none of the equipment used was suitable for direct visualization of the pore space in fine-grained structures such as those found in shales; fractures, discontinuities, and millimeter scale features were readily detectable with the methods tested. Imaging with the NETL medical CT scanner was performed on the entire core. Qualitative analysis of the medical CT images, coupled with X-ray fluorescence (XRF), P-wave, and magnetic susceptibility measurements from the MSCL were useful in identifying zones of interest for more detailed analysis. A selection of samples (Table 1) were cored, sliced, and powdered for additional characterization analyses. These analyses did involve destructive subsampling of the full core at discrete sections, and the results are presented here in the context of the larger core description. Selected sections of the core were removed from the full core for detailed analyses using the following destructive techniques: bulk inductively coupled plasma-optical emission spectroscopy (ICP-OES), isolation of carbon and sulfur, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and higher resolution CT scan with NETL’s micro-CT scanning systems. The ability to quickly identify key areas for more detailed study with higher resolution will save time and resources in future studies. The combination of methods used provides a multi-scale analysis of the core; the resulting macro and micro descriptions are relevant to many subsurface energy related examinations traditionally performed at NETL.

04 OIL SHALES AND TAR SANDS↗

IACMI Project 4.2: Thermoplastic Composite Development for Wind Turbine Blades

(Section 5.1) Composites made from Arkema’s Elium® thermoplastic resin and Johns Manville fiberglass were researched during this project for applications in wind blade manufacturing. A techno-economic model was developed to model this wind blade manufacturing process using these materials in place of traditional composites made with thermoset resin. This model was based on manufacturing a 61.5-meter wind blade, which showed a 4.7% reduction in wind blade cost as compared traditional thermoset materials. These cost savings were not from the thermoplastic material costing less than traditional thermoset materials, but rather from decreased capital costs, faster cycle times and reduced energy requirements and labor costs. (Section 5.2) An infusion and curing model was developed for thermoplastic composite wind blades using PAM-RTM. The primary goal was to demonstrate the infusion simulation for the Elium® resin system on a 13-meter wind blade. Additionally, the exotherm temperature was predicted and compared to measurements, which showed model results within 10% of actual measurements. (Section 5.3) Composite laminate panels and composite sandwich panels with a balsa core were produced; specimens were cut and characterized. Similar composite specimens were made with Elium® thermoplastic resin and Hexion thermoset epoxy (RIMR135/RIMH1366) to enable comparisons between these resin systems. The static test methods included: tensile, compression, in-plane shear, interlaminar shear, flexural, sandwich core shear flexure, and single cantilever beam tests for sandwich beams. Fatigue testing at room temperature was completed to composite laminate panels at a stress ratio of R=0.1 and R=10. In addition, fatigue testing to laminate panels was completed at -30°C, and at room temperature after conditioning specimens at 70°C and 90% relative humidity. Overall, mechanical test results from Elium® composites are similar to epoxy composites. (Section 5.4) Elium composite panels were produced with intentional defects such as voids and nonwetting of fibers to begin to understand performance sensitivity to defects. A thermal digital image correlation (TDIC) method provides high spatial resolution strain field at elevated temperatures and can be used to identify defective regions within composite panels. Flexural modulus differences of 21% were seen between defect and non-defect panels. Other Elium® composite panels were forced to be defective by boiling the resin after infusion, which created voids throughout the composite laminate. X-ray computed tomography scanning was used to view the internal structure of the defect panels. Defect panels had a significant reduction in fatigue life as compared to baseline panels produced without intentional defects. (Section 5.5) Lap shear specimens were fabricated to compare the lap shear strength of an off-the-shelf adhesive (Plexus MA590) and two new adhesives developed by Arkema (Bostik SAF30 90 and Bostik SAF30 120). ISO standard 4587:2003 was used to standardize the testing method and sample fabrication. Lap shear specimens were made at 1mm, 3mm, and 10mm thicknesses. The Bostik adhesive lap shear test results were similar to Plexus for all thicknesses. (Section 5.6) Fiber-reinforced polymer (FRP) composites are typically used in high-performance applications (e.g., aerospace), and their expansion into high-volume industries (e.g. consumer automotive and wind turbine blade manufacturer or similar) is hindered by their cost and a lack of efficient manufacturing techniques. Monitoring the curing process of these composites during manufacturing can improve the efficiency of the process, and therefore reduce the manufacturing cost. Cure monitoring techniques were developed that use probabilistic estimation methods and surface temperature measurements made using infrared cameras. These techniques enable real-time monitoring of the infusion process to locate manufacturing flaws, and they can, potentially, estimate residual stresses in the part. Their commercialization will help facilitate expansion of FRP composites in high-volume industries. (Section 5.7) A 13-meter composite wind blade was produced with Elium® resin and Johns Manville fiberglass; this blade was made with VARTM processing similar to how megawatt-scale wind blades are currently manufactured, but no post-mold heating was used for this thermoplastic composite blade. The wind blade underwent full-scale validation for static loading (4-different load orientations) and flapwise fatigue loading to simulate 20-years of operational loads. The thermoplastic composite wind blade withstood the loading without any noted issues and performed similar to results from a previous full-scale validation to an equivalent epoxy composite wind blade produced with the same blade molds. (Section 5.8) A study was conducted to determine the feasibility of recycling composite wind turbine blade components fabricated with glass fiber reinforced Elium® thermoplastic resin. Dissolution, which is a process unique to thermoplastic matrices, allows recovery of both the polymer matrix and full-length glass fibers, while maintaining their stiffness and strength throughout the recovery process. The economics of recycling is favorable if 50% of the glass fiber is recovered and resold for a process of $\$$ 0.28/kg, and 90% of the resin is recovered and resold at a price of $\$$ 2.50/kg.(Section 10) Recommendations are outlined for commercializing thermoplastic resin for composite wind blade production, in addition to recommended areas for future research.

17 WIND ENERGY↗

Collective Summary of sCO2 Materials Development (Supercritical Transformational Electric Power Generation (STEP) Level 2 Milestone Report) (Parts I - II)

Polymers such as PTFE (polytetrafluorethylene or Teflon), EPDM (ethylene propylene diene monomer) rubber, FKM fluoroelastomer (Viton), Nylon 11, Nitrile butadiene (NBR) rubber, hydrogenated nitrile rubber (HNBR) and perfluoroelastomers (FF_202) are commonly employed in super critical CO 2 (sCO2) energy conversion systems. O-rings and gaskets made from these polymers face stringent performance conditions such as elevated temperatures, high pressures, pollutants, and corrosive humid environments. In FY 2019, we conducted experiments at high temperatures (100°C and 120°C) under isobaric conditions (20 MPa). Findings showed that elevated temperatures accelerated degradation of polymers in sCO2, and that certain polymer microstructures are more susceptible to degradation over others. In FY 2020, the focus was to understand the effect of sCO2 on polymers at low (10 MPa) and high pressures (40 MPa) under isothermal conditions (100°C). It was clear that the same selectivity was observed in these experiments wherein certain polymeric functionalities showed more propensity to failure over others. Fast diffusion, supported by higher pressures and long exposure times (1000 hours) at the test temperature, caused increased damage in sCO2 environments to even the most robust polymers. We also looked at polymers under compression in sCO2 at 100°C and 20 MPa pressure to imitate actual sealing performance required of these materials in sCO2 systems. Compression worsened the physical damage that resulted from chemical attack of the polymers under these test conditions. In FY 2021, the effect of cycling temperature (from 50°C to 150°C to 50°C) for polymers under a steady sCO2 pressure of 20 MPa was studied. The aim was to understand the influence of cycling temperatures of sCO2 for typical polymers under isobaric (20 MPa) conditions. Thermoplastic polymers (Nylon, and PTFE) and elastomers (EPDM, Viton, Buna N, Neoprene, FF202, and HNBR) were subjected to 20 MPa sCO2 pressure for 50 cycles and 100 cycles in separate experiments. Samples were extracted for ex-situ characterization at 50 cycles and upon the completion of 100 cycles. Each cycle constituted of 175 minutes of cycling from 50°C to 150°C. The polymer samples were examined for physical and chemical changes by Dynamic Mechanical and Thermal Analysis (DMTA), Fourier Transform Infrared (FTIR) spectroscopy, and compression set. Density and mass changes immediately after removal from test were measured for degree of swell comparisons. Optical microscopy techniques and micro computer tomography (micro CT) images were collected on select specimens. Evaluations conducted showed that exposures to super-critical CO2 environments resulted in combinations of physical and/or chemical changes. For each polymer, the dominance of cycling temperatures under sCO2 pressures, were evaluated. Attempts were made to qualitatively link the permanent sCO2 effects to polymer micro- structure, free volume, backbone substitutions, presence of polar groups, and degree of crystallinity differences. This study has established that soft polymeric materials are conducive to failure in sCO2 through mechanisms of failure that are dependent on polymer microstructure and chemistry. Polar pendant groups, large atom substitutions on the backbone are some of the factors that are influential structural factors.

36 MATERIALS SCIENCE↗

X-ray CT Scans - Molluscs - Set 1

A collection of x-ray computed tomography scans of specimens from the Bailey-Matthews National Shell Museum.

59 BASIC BIOLOGICAL SCIENCES↗

X-ray CT Scans - Molluscs - Set 2

A collection of x-ray computed tomography scans of specimens from the Denver Museum of Nature & Science.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

X-ray CT Scans - Rodents - Set 4

A collection of x-ray computed tomography scans of specimens from the Museum of Southwestern Biology.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

X-Ray CT Scans - Rodents Set 5

A collection of x-ray computed tomography scans of specimens from the Museum of Southwestern Biology.

59 BASIC BIOLOGICAL SCIENCES↗

Clean Condensing Gas Furnace

Natural gas furnaces are the most common space heating equipment in the U.S. residential and commercial building markets. However, current residential natural gas condensing furnaces generate substantial acidic condensate as well as significant emissions of sulfur oxides (SOx), nitrogen oxides (NOx), carbon monoxide (CO), hydrocarbons (HC), and methane (CH 4 ) contributing to environmental degradation of air, water, and soil. This report describes a novel solution to reduce the environmental impact of natural gas condensing furnaces based on the technology of a monolithic acidic gas reduction (AGR) catalyst for SOx trapping, NOx redox to nitrogen, and oxidation of formic acid, CO, HC, and CH 4 . The AGR technology offers the following benefits: (1) a neutral furnace condensate with a pH of ~7, allowing its safe release into the sewer system thus eliminating a second drainage system; (2) trapping and removing nearly all SOx emissions; (3) NOx emissions nearly at nearly 1-2 ng/J, more than 95% lower than new emissions standards in California; (4) the use of a low-cost heat exchanger as a condensing heat exchanger (HX) since the condensate is not acidic, avoiding the need for expensive stainless steel alloys; and (5) unburnt fuel energy recovery to boost efficiency.The AGR component and AGR-enabled furnace performance were broadly tested to determine their effects on long-term reliability and durability, as well as SOx storage and regeneration activity. The AGR regeneration does not impair the performance in achieving neutral condensate and ultra-low NOx emissions, and the AGR catalyst subjected to regeneration activities continued to function well and achieved slightly better annual fuel utilization efficiency (AFUE). The 400-hour reliability and durability test of the retrofitted condensing furnace with the AGR component shows that the furnace unit still achieves a neutral furnace condensate with a pH of ~7 and enables 0~3 ng/J of NOx emissions. However, the 400-hour operation slightly degraded the AFUE because of soot particle accumulation caused by frequent incomplete combustion owing to inappropriate condensate drainage during testing. Thus, proper condensate drainage is critical for AGR-enabled furnaces. Furthermore, neutron computed tomography was employed to survey the aged AGR component and demonstrate high-resolution 2D and 3D representations for the nondestructive diagnosis of the AGR component. The tomography showed that the AGR component did not deform or suffer broken AGR channels. A new AGR catalyst with low precious metal loading was preliminarily explored to identify a pathway of optimizing AGR material loading and maximizing acidic gas reduction at low cost. The new AGR component can reduce precious metal loading by 38% and still achieve neutral condensate and ultralow NOx emissions. The furnace with the AGR component of low Pt/Rh loading enables a maximum AFUE of 97%, which is meaningfully higher than the original furnace. Long-duration testing for the furnace enabled with the low precious metal loading AGR component will be vital in future research. Although the current work demonstrates a proof of concept for the AGR-enabled furnace, the AGR assembly needs to be optimized and integrated into the design of new OEM furnace products. Furthermore, the AGR technology can be applied not only for residential gas furnaces, but also for commercial rooftop units, gas heat pumps, gas-fired water heaters, combustion boilers, and other systems.

03 NATURAL GAS↗

Technology Enabling Zero-EPZ Micro Modular Reactors: Fabrication of Zirconium Hydride with Controlled Hydrogen Loading

This report completes Milestone M2.2.2 - ZrH pellet fabricated with controlled hydride loading: ZrH1.5±0.1 single phase pellets fabricated with controlled and thermally stable hydride loading. Hydrogen content to be quantified and single-phase confirmed by X-ray diffraction. In this milestone, we report the successful fabrication of delta-phase zirconium hydride pellets using the ORNL bulk metal hydriding system. The successful deployment of zirconium hydride moderator in advanced reactors requires development of a consistent and affordable production pathway along with implementation of a hydrogen retention solution throughout the reactor life. Fabrication of delta-phase zirconium hydride is challenging since the absorption of a large amount of hydrogen into alpha-zirconium induces significant volume expansion and the present hydrogen concentration gradient results in cracking. A fully programmable hydriding system with continuous hydrogen partial pressure and flow control to facilitate processing of massive metal hydride has been developed at ORNL. In this report, the working principle of the hydriding system will be introduced. Characterization of the produced zirconium hydride includes X-ray powder diffraction to identify the present phases and X-ray Computed Tomography to visualize the internal microstructure (including cracks). The results indicate that single delta-phase zirconium hydride pellets with various sizes have been successfully produced.

36 MATERIALS SCIENCE↗

In-Situ Spatial Mapping of Hydrogen in Yttrium Hydrides at LANSCE

This report summarizes the neutron imaging techniques and experimental activities performed at the Los Alamos Neutron Science Center (LANSCE) with the main goal of measuring temperature driven hydrogen diffusion within bulk-yttrium hydride (YH x ) materials. The experimental results and technique developments reported herein support the US Department of Energy Office of Nuclear Energy’s (DOE-NE) Microreactor Program under Technology Maturation. In particular, the critical need to experimentally validate and verify hydrogen-diffusion models of metal hydrides used in hightemperature microreactor designs is addressed by means of high-spatial-resolution neutron imaging coupled with custom-built and application-specific furnaces. These capabilities were designed to apply large temperature gradients across centimeter-sized YH x pellets to simulate conditions faced in the microreactor environment. Neutron imaging, combined with in-situ sample heating, enables near real-time tracking of hydrogen diffusion in YH x on the sub-millimeter scale. In this report, an overview of neutron imaging methodology and technologies are given in the context of recent spatial measures of hydrogen concentrations in similar metals hydrides. Additionally, the commissioning and operation of a custom-built compact dual-zone furnace is given along with details on the first two in-situ heating measurements of YH x performed over the 2020 and 2021 LANSCE operation cycles. In parallel with in-situ heating measurements, neutron computed tomography scans were performed to visualize hydrogen aggregates in post-heated YH x samples. Analysis and results from these neutron imaging measurements are given along with outlooks and plans for improving future hydrogen diffusion measurements at LANSCE.

47 OTHER INSTRUMENTATION↗

Quantification of morphological change in materials based on image data utilizing machine learning techniques

Computed tomography (CT) resolution has become high enough to monitor morphological changes due to aging in materials in long-term applications. We explored the utility of the critic of a generative adversarial network (GAN) to automatically detect such changes. The GAN was trained with images of pristine Pharmatose, which is used as a surrogate energetic material. It is important to note that images of the material with altered morphology were only used during the test phase. The GAN-generated images visually reproduced the microstructure of Pharmatose well, although some unrealistic particle fusion was seen. Calculated morphological metrics (volume fraction, interfacial line length, and local thickness) for the synthetic images also showed good agreement with the training data, albeit with signs of mode collapse in the interfacial line length. While the critic exposed changes in particle size, it showed limited ability to distinguish images by particle shape. The detection of shape differences was also a more challenging task for the selected morphological metrics that related to energetic material performance. We further tested the critic with images of aged Pharmatose. Subtle changes due to aging are difficult for the human analyst to detect. Both critic and morphological metrics analysis showed image differentiation.

36 MATERIALS SCIENCE↗

Understanding Phase and Interfacial Effects of Spall Fracture in Additively Manufactured Ti-5Al-5V-5Mo-3Cr

Additive manufactured Ti-5Al-5V-5Mo-3Cr (Ti-5553) is being considered as an AM repair material for engineering applications because of its superior strength properties compared to other titanium alloys. Here, we describe the failure mechanisms observed through computed tomography, electron backscatter diffraction (EBSD), and scanning electron microscopy (SEM) of spall damage as a result of tensile failure in as-built and annealed Ti-5553. We also investigate the phase stability in native powder, as-built and annealed Ti-5553 through diamond anvil cell (DAC) and ramp compression experiments. We then explore the effect of tensile loading on a sample containing an interface between a Ti-6Al-V4 (Ti-64) baseplate and additively manufactured Ti-5553 layer. Post-mortem materials characterization showed spallation occurred in regions of initial porosity and the interface provides a nucleation site for spall damage below the spall strength of Ti-5553. Preliminary peridynamics modeling of the dynamic experiments is described. Finally, we discuss further development of Stochastic Parallel PARticle Kinteic Simulator (SPPARKS) Monte Carlo (MC) capabilities to include the integration of alpha (α)-phase and microstructural simulations for this multiphase titanium alloy.

36 MATERIALS SCIENCE↗