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Subtask 1.3 – Integrated Carbon Capture and Storage for North Dakota Ethanol Production

The Energy & Environmental Research Center (EERC), in partnership with Red Trail Energy, LLC (RTE), a North Dakota ethanol producer; the North Dakota Industrial Commission (NDIC) Renewable Energy Program (REP); and the U.S. Department of Energy (DOE), conducted a feasibility and implementation study for a commercial carbon capture and storage (CCS) effort. This subtask provided technical support and developed recommended practices of how small-scale industrial CO2 emitters (<1,000,000 tonnes of CO2 emitted annually) may economically deploy CCS. The 64-million-gallon dry mill RTE ethanol facility, emitting an average 180,000 tonnes of CO2 annually, was the subject of the case study. The positive outcome of this research, which shows technical and economic potential for ethanol–CCS in North Dakota, has resulted in RTE acquiring an approved Permit to Drill on December 2, 2019, for a stratigraphic test well in early 2020, a necessary step toward a North Dakota CO2 Storage Facility Permit (SFP) for the RTE CCS effort. Outcomes include 1) validating the Broom Creek Formation as a regional target for CCS, 2) determining the full carbon life cycle of an industrial fuel production facility with CCS, 3) developing a field implementation plan (FIP) for small-scale CCS, and 4) determining the validity and pathway for using CCS to meet low-carbon fuel (LCF) standards. The technical team included the EERC, RTE, Trimeric Corporation, Schlumberger Carbon Services, and Computer Modelling Group (CMG). Findings from activities conducted November 2016 – May 2020 are summarized as follows. Several key steps have been accomplished toward validating the Broom Creek Formation as a CO2 injection and storage target at the RTE CCS site, including verification of the presence and structure of sandstone layers that may comprise the potential CO2 storage reservoir and the several thousand feet of overlying confining zone. Work included site characterization using existing data, interpretation of seismic data within the study area, and geologic modeling simulation of CO2 injection. Interpreted results estimate 3000 feet of confining zone between the Broom Creek Formation (storage target) and the lowermost underground source of drinking water (e.g., the Fox Hills Formation). The thickness of the Broom Creek injection target varies 230–420 ft within the survey area. Results were used to inform the location of a stratigraphic test well and associated characterization test program. No impediments were identified within the targeted CO2 storage complex that would prevent the project from moving forward. A stratigraphic test well is the next step to validate these results and to acquire remaining data necessary to develop a North Dakota CO2 SFP application. The EERC generated full carbon life cycle estimates for CCS integration with the RTE ethanol facility. Results indicated that an average 40% reduction in CO2 emissions is possible through CCS implementation. Approximately half of the carbon in the overall life cycle for a dry mill ethanol plant is generated through the fermentation process and emitted to the atmosphere; this is the CO2 stream targeted for CCS. The remaining carbon is attributed to corn feedstock farming (diesel, fertilizer), energy for fuel processing (natural gas, electricity), and transportation (diesel) of the fuel product. Life cycle carbon estimates are also affected by the anticipated energy consumption of a potential capture facility, which depend on the type of CO2 product generated. For example, a 30%–40% net CO2 emission reduction is estimated if a liquefied CO2 facility were incorporated compared to a 40%–50% net CO2 reduction if a supercritical “injection-grade” CO2 product is generated; i.e., more energy is required to further refine the CO2 stream, affecting the full carbon life cycle estimates. A CCS FIP was developed and initiated at the RTE CCS site, resulting in the development of several guidance documents: a CO2 Capture Process Design Package, a North Dakota CO2 geologic Storage Permits Template, and a Public Outreach Package for CCS in North Dakota. General FIP components include CO2 capture system, pipeline and well designs; monitoring, verification, and accounting (MVA) plans; geologic characterization and testing programs; and permitting and outreach plans. Vendor bids were also acquired for the CO2 liquefaction facility. Near-surface characterization (groundwater and soil gas sampling) and geologic characterization (seismic survey) were initiated to inform development of a UIC Class VI-compliant MVA plan compliant with a North Dakota CO2 SFP. Designs (well and geologic testing) were completed for a stratigraphic test well compliant with a North Dakota CO2 SFP. In addition, the outreach plan was executed, including community open houses, meetings with city/county/state officials, and development of public materials. Although other entities continued to mature incentive programs in 2019–2020, California and the Internal Revenue Service (IRS) currently provide the most advanced economic opportunities for CCS integrated with fuel production. The California Low-Carbon Fuel Standard (LCFS) adopted a CCS Protocol in January 2019, allowing submittal of a design-based pathway (DBP) application for an approved temporary (not certified) carbon intensity value for a fully engineered facility. An ethanol–CCS DBP application to the California LCFS Program (officially approved February 28, 2020) was developed to show that the RTE CCS effort meets LCFS requirements. The approved DBP provides confidence to advance the project and supports potential investments. Other entities continue to mature incentive programs. The IRS issued guidance in February 2020 that addresses the definition of beginning of construction and revenue procedure on partnerships for the Enhancement of Carbon Dioxide Sequestration Credit (a.k.a. Section 45Q) CCS tax credit program; the IRS anticipates issuing further guidance on issues such as secure geologic storage, utilization qualifications, and recapture of claimed credits. Maturing incentive programs coupled with workable permitting regulations provide confidence to advance CCS projects in North Dakota and support financial investment to proceed with designing, constructing, and implementing CCS projects at small-scale fuel production facilities. The largest hurdles for CCS implementation at small-scale industrial systems are often business/economic-related (i.e., not technical). Market uncertainty already exists for agriculture-based alternative fuels such as corn ethanol, for which production has increased by ~33%, and prices have correspondingly lowered since 2015. Passing the Section 45Q tax credit program improves economic feasibility for CCS but may require external investors for a small business to achieve maximum benefits. Public–private partnerships with NDIC and DOE have resulted in foundational technical and regulatory knowledge, growing stakeholder confidence, and a pathway to implementation that enables similar industrial CCS projects in the region to advance. This subtask was funded through the EERC–DOE Joint Program on Research and Development for Fossil Energy-Related Resources Cooperative Agreement No. DE-FE0024233. Nonfederal funding was provided by NDIC and RTE. The authors would also like to thank CMG, ESRI, IHS, Neuralog, and Schlumberger for allowing the use of their software packages in support of this work.

42 ENGINEERING↗

Effect of Stoichiometry on the Structure and Polarization of BaTiO 3

Barium titanate (BaTiO 3 ) is a material of interest for photonic device applications due to its strong optical non-linearity. However, BaTiO 3 -based devices have not found widespread adoption, in part due to the challenges associated with synthesizing high quality thin-films. Here, high-resolution scanning transmission electron microscope (STEM) imaging is used to investigate the atomic structure of both on- and off-stoichiometric BaTiO 3 synthesized by molecular beam epitaxy (MBE). Here, this investigation reveals an asymmetry in the way the BaTiO 3 atomic lattice accommodates off-stoichiometry growth and unveils features beyond what is expected from diffraction or surface characterization techniques. Excess titanium incorporates into the BaTiO 3 lattice to form pervasive defects despite titanium-rich films having a low surface roughness and high-quality appearance in diffraction. Excess barium forms a rough, water-soluble surface layer but does not significantly impact the quality of the BaTiO 3 lattice. STEM is used to map titanium atom displacement in real-space. The average displacement distance is 30–60 pm in the strained thin-films, higher than the <20 pm displacement in bulk BaTiO 3 . Additionally, the titanium atom displacement direction deviates from the c-axis of the unit cell, which may have implications for the material's electro-optic tensor and thus for electro-optic device design.

Cavanagh, Ashley E. [Harvard Univ., Cambridge, MA ↗

A semiempirical model for interpreting microwave emission from semiarid land surfaces as seen from space

A radiative-transfer model for simulating microwave brightness temperatures over land surfaces is described. The model takes into account sensor viewing conditions (spacecraft altitude, viewing angle, frequency, and polarization) and atmospheric parameters over a soil surface characterized by its moisture, roughness, and temperature and covered with a layer of vegetation characterized by its temperature, water content, single scattering albedo, structure, and percent coverage. In order to reduce the influence of atmospheric and surface temperature effects, the brightness temperatures are expressed as polarization ratios that depend primarily on the soil moisture and roughness, canopy water content, and percentage of cover. The sensitivity of the polarization ratio to these parameters is investigated. Simulation of the temporal evolution of the microwave signal over semiarid areas in the African Sahel is presented and compared to actual satellite data from the SMMR instrument on Nimbus-7.

Kerr, Yann H.↗

Mars Array Technology Experiment Developed to Test Solar Arrays on Mars

Solar arrays will be the power supply for future missions to the planet Mars, including landers, rovers, and eventually human missions to explore the Martian surface. Until Mars Pathfinder landed in July 1997, no solar array had been used on the surface. The MATE package is intended to measure the solar energy reaching the surface, characterize the Martian environment to gather the baseline information required for designing power systems for long-duration missions, and to quantify the performance and degradation of advanced solar cells on the Martian surface. To measure the properties of sunlight reaching the Martian surface, MATE incorporates two radiometers and a visible/NIR spectrometer. The radiometers consist of multiple thermocouple junctions using thin-film technology. These devices generate a voltage proportional to the solar intensity. One radiometer measures the global broadband solar intensity, including both the direct and scattered sunlight, with a field of view of approximately 130. The second radiometer incorporates a slit to measure the direct (unscattered) intensity radiation. The direct radiometer can only be read once per day, with the Sun passing over the slit. The spectrometer measures the global solar spectrum with two 256-element photodiode arrays, one Si sensitive in the visible range (300 to 1100 nm), and a second InGaAs sensitive to the near infrared (900 to 1700 nm). This range covers 86 percent of the total energy from the Sun, with approximately 5-nm resolution. Each photodiode array has its own fiber-optic feed and grating. Although the purpose of the MATE is to gather data useful in designing solar arrays for Mars surface power systems, the radiometer and spectrometer measurements are expected to also provide important scientific data for characterizing the properties of suspended atmospheric dust. In addition to measuring the solar environment of Mars, MATE will measure the performance of five different individual solar cell types and two different solar cell strings, to qualify advanced solar cell types for future Mars missions. The MATE instrument, designed for the Mars-2001 Surveyor Lander mission, contains a capable suite of sensors that will provide both scientific information as well as important engineering data on the operation of solar power systems on Mars. MATE will characterize the intensity and spectrum of the solar radiation on Mars and measure the performance of solar arrays in the Mars environment. MATE flight hardware was built and tested at the NASA Glenn Research Center and is ready for flight.

Landis, Geoffrey A.↗

Machine-learning-based automatic small-angle measurement between planar surfaces in interferometer images: A 2D multilayer Laue lenses case

Here, we report a new machine-learning-based approach to automatically measure the small angle between multiple planar surfaces characterized by white light interferometers. By applying an unsupervised clustering algorithm, DBSCAN (Density-Based Spatial Clustering of Applications with Noise), the multiple surfaces in an interferometer image are automatically identified as distinct surfaces. The angles between every two surfaces are then calculated through the surface fitting. This method can be applied to multiple surfaces regardless of their shapes and locations and significantly simplifies the angle measurement procedure. Using the developed method, we have demonstrated a quick and precise angle measurement for the alignment of 2D Multilayer Laue Lenses (MLLs) for the development of high-resolution x-ray microscopy. This automatic, accurate, and robust small-angle measurement method is compatible with widely used white light interferometers and can be further applied to other metrology applications of interferometer results.

36 MATERIALS SCIENCE↗

Evaluation of high temperature structural adhesives for extended service

Eight different Ti-6Al-4V surface treatments were investigated for each of 10 candidate resins. Primers (two for each resin) were studied for appropriate cure and thickness and initial evaluation of bond joints began using various combinations of the adhesive resins and surface treatments. Surface failure areas of bonded titanium coupons were analyzed by electron microscopy and surface chemical analysis techniques. Results of surface characterization and failure analysis are described for lap shear bond joints occurring with adhesive systems consisting of: (1) LARC-13 adhesive, Pasa jell surface treatment; (2) LARC-13 adhesive, 10 volt CAA treatment; (3) PPQ adhesive, 10 volt CAA treatment; and (4) PPQ adhesive, 5 volt CAA treatment. The failure analysis concentrated on the 10,000 hr 505K (450 F) exposed specimens which exhibited adhesive failure. Environmental exposure data being generated on the PPQ-10 volt CAA and the LARC-TPI-10 volt CAA adhesive systems is included.

Hill, S. G.↗

Decoupling plasma, catalyst, and gaseous mechanisms for non-oxidative methane conversion

Direct non-oxidative methane (CH 4 ) conversion to value-added hydrogen (H 2 ) and C 2 products remains hindered by fundamental catalytic scaling constraints and rapid surface deactivation at elevated temperatures. Plasma-enabled catalysis offers a promising route to overcome the thermodynamic and kinetic barriers of direct non-oxidative methane upgrading at mild conditions, yet control over C–C product selectivity and catalyst stability remains elusive. Here, we establish a unified mechanistic framework including Langmuir–Hinshelwood (L–H) and Langmuir–Rideal (L–R) mechanisms that disentangles the roles of plasma excitation (including vibrationally activated species and radicals), surface temperature (T sur ), and catalyst binding energy in steering CH 4 conversion to H 2 and C 2 hydrocarbons. Through a combination of density functional theory (DFT) informed microkinetic modeling, in situ and ex situ surface characterization, and product quantification under dielectric barrier discharge conditions, we show that vibrationally excited CH 4 lowers activation barriers selectively for dissociative chemisorption, enabling surface activation across a wide range of transition metal catalysts at low thermal energy input. We find that once CH 4 is dissociatively chemisorbed, the branching between C 2 H 2 , C 2 H 4 , and C 2 H 6 is governed by surface properties (carbon binding energy, T sur , etc), regardless of plasma excitation. The DFT informed microkinetic model decouples the effects of molecular activation from surface properties and indentifies operating windows that maximize target yields while suppressing carbon accumulation and subsequent catalytic inactivation. Experiments on polycrystalline Cu/Al 2 O 3 , Ni/Al 2 O 3 , and Pt/Al 2 O 3 validate these predictions, revealing catalyst-dependent branching toward ethane or ethylene and distinct deactivation profiles. We unify these trends into a generalized three-dimensional plasma-thermal-catalytic design space, from which reduced descriptors such as T vib /T sur in the limit of vibrationally excited L–H pathways emerge as predictive metrics. These results enable rational tuning of methane conversion pathways and unlock selective C 2 formation using earth-abundant metals under mild plasma conditions.

catalyst inactivation↗

Determination of high temperature strains using a PC based vision system

With the widespread availability of video digitizers and cheap personal computers, the use of computer vision as an experimental tool is becoming common place. These systems are being used to make a wide variety of measurements that range from simple surface characterization to velocity profiles. The Sub-Pixel Digital Image Correlation technique has been developed to measure full field displacement and gradients of the surface of an object subjected to a driving force. The technique has shown its utility by measuring the deformation and movement of objects that range from simple translation to fluid velocity profiles to crack tip deformation of solid rocket fuel. This technique has recently been improved and used to measure the surface displacement field of an object at high temperature. The development of a PC based Sub-Pixel Digital Image Correlation system has yielded an accurate and easy to use system for measuring surface displacements and gradients. Experiments have been performed to show the system is viable for measuring thermal strain.

Mcneill, Stephen R.↗

Polarimetric backscattering from sea ice

Polarimetric backscattering from sea ice is presented. Theoretical models for backscattering are first presented for various ice types. Then, theoretical results are compared with experimental data for new thin ice, first-year ice, and multi-year ice. Sea ice is modeled as a layer medium containing random scatterers and rough interfaces. For multi-year sea ice with snow cover, the sea ice layer is modeled as an ice background with embedded spheroidal air bubbles and the snow layer as air with ice grains. The hummocky topography on multi-year ice is characterized by a Gaussian distribution which has an averaging effect on backscattering coefficients. First-year sea ice is described by an ice medium hosting ellipsoidal brine inclusions. These inclusions are oriented preferentially in the vertical direction due to the columnar structure of first-year sea ice. Azimuthally, the orientation of the brine pockets are random corresponding to the random c-axes in sea ice, unless the axes are oriented by sea currents. For thin ice in newly opened leads, it has been observed that there exists a thin brine layer with very high salinity on the top surface of the new ice. This brine layer is depicted as a medium with high permittivity which can significantly affect electromagnetic scattering signatures from the lower thin ice layer, with a higher fractional volume of brine inclusions due to higher salinity as compared to thick first-year sea ice. The rough medium interfaces are described as Gaussian rough surfaces characterized by root-mean-square heights and surface correlation lengths. The contribution from rough surface, calculated under the Kirchhoff approximation or small perturbation method, is assumed to be independent from volume scattering. The total loss including absorption and scattering losses in the scattering media is represented by the imaginary part of effective permittivity obtained from the strong fluctuation theory. The polarimetric scattering coefficients for different ice types are then derived under the distorted Born approximation.

Nghiem, S. V.↗

Effectiveness of Surface Treatment Techniques for Composite Bonding with Different Contamination Levels

Various surface treatment techniques have been developed to promote adhesive bond performance for composite structural components in aerospace applications. The condition of the pre-bond surface is critical to achieving desirable bond quality. Contamination on bonding surfaces is well recognized as a major threat to ultimate bond performance. Variation in contamination level has brought additional challenges into manufacturing process control. High fidelity surface treatment techniques are required for effective removal of contaminants over a wide range of contamination levels. In this study, a common contaminant, i.e. silicone mold release, was introduced to pre-bond composite surfaces with different concentrations. Plasma and laser surface treatment techniques were performed and their effectiveness in restoring and enhancing desirable bond quality was investigated. Surface characterization techniques, including water contact angle goniometry, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy, were conducted to assess the condition of contaminated surfaces and the improvement induced by plasma and laser surface treatments. Failure modes from a customized double cantilever beam test were investigated before and after surface treatments. Fundamental mechanisms of plasma and laser surface treatments on the composite bonding surfaces were also investigated.

Fang, Xiaomei↗

Wildfire Risk Support via Satellite-Derived Vegetation Health and Land Surface Model Soil Moisture

Land Surface Model (LSM) and evaporative demand products provide advanced lead time to wildfire conditions that complement traditional fire indices and represent short-term changes that add context to overall, long-term drought conditions. Established fire indices typically use weather indicators (i.e., precipitation, temperature) and estimated dead fuel moisture to indirectly obtain land surface and sub-surface characterization. The convergence of LSM shallow and deep-layer soil moisture output and satellite-derived vegetation health combine to provide a tool for stakeholders to examine trends in the state of land surface conditions that can help assess wildfire threat. Satellite remote sensing data can constrain near-real time vegetation characteristics within the LSM and/or provide a derived stress index in order to help characterize the wildfire risk. In addition, a percentile product of soil moisture is derived from a comparison of current LSM conditions to the historical record of the LSM in order to put the current conditions in perspective relative to the season and geographic region. The 2015 season as well as the 2018 Camp Fire Complex in California were examined in terms of the changes in LSM soil moisture and vegetation states. Satellite vegetation health consistently showed decreases a month prior to wildfire initiation. Additionally, maximum changes in total column soil moisture corresponded with the greatest concentration of fire locations. While soil moisture deficits occurred in the shallow layers across northern California in 2018, significant deficits at all sub-surface levels were seen ahead of the Camp Fire event. This presentation will demonstrate the complementary value of LSM output and satellite measured vegetation health to diagnose short-term deficits in sub-surface soil moisture and the rapid decline in vegetation health which precedes large wildfire events.

Wildfire↗

Atomic structure of different surface terminations of polycrystalline ZnPd

The intermetallic compound ZnPd has been found to have desirable characteristics as a catalyst for the steam reforming of methanol. The understanding of the surface structure of ZnPd is important to optimize its catalytic behavior. However, due to the lack of bulk single-crystal samples and the complexity of characterizing surface properties in the available polycrystalline samples using common experimental techniques, all previous surface science studies of this compound have been performed on surface alloy samples formed through thin-film deposition. In this study, we present findings on the chemical and atomic structure of the surfaces of bulk polycrystalline ZnPd studied by a variety of complementary experimental techniques, including scanning tunneling microscopy (STM), x-ray photoelectron spectroscopy (XPS), low energy electron microscopy (LEEM), photoemission electron microscopy (PEEM), and microspot low-energy electron diffraction ( μ -LEED). These experimental techniques, combined with density functional theory (DFT)-based thermodynamic calculations of surface free energy and detachment kinetics at the step edges, confirm that surfaces terminated by atomic layers composed of both Zn and Pd atoms are more stable than those terminated by only Zn or Pd layers. DFT calculations also demonstrate that the primary contribution to the tunneling current arises from Pd atoms, in agreement with the STM results. The formation of intermetallics at surfaces may contribute to the superior catalyst properties of ZnPd over Zn or Pd elemental counterparts. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗

Extreme ultraviolet microscope characterization using photomask surface roughness

We demonstrate a method for characterizing the field-dependent aberrations of a full-field synchrotron-based extreme ultraviolet microscope. The statistical uniformity of the inherent, atomic-scale roughness of readily-available photomask blanks enables a self-calibrating computational procedure using images acquired under standard operation. We characterize the aberrations across a 30-um field-of-view, demonstrating a minimum aberration magnitude of smaller than λ/21 rms averaged over the center 5-um area, with a measurement accuracy better than λ/180 rms. The measured field variation of aberrations is consistent with system geometry and agrees with prior characterizations of the same system. In certain cases, it may be possible to additionally recover the illumination wavefront from the same images. Our method is general and is easily applied to coherent imaging systems with steerable illumination without requiring invasive hardware or custom test objects; hence, it provides substantial benefits when characterizing microscopes and high-resolution imaging systems in situ.

47 OTHER INSTRUMENTATION↗

Unraveling the Mechanism of Water-Mediated Sulfur Tolerance via Operando Surface-Enhanced Raman Spectroscopy

While several proton-conducting anode materials have shown excellent tolerance to sulfur poisoning, the mechanism is still unclear due largely to the inability to probe miniscule amounts of sulfur-containing species using conventional surface characterization techniques. Here we present our findings in unraveling the mechanism of water-mediated sulfur tolerance of a proton conductor under operating conditions empowered by surface-sensitive, operando surface-enhanced Raman spectroscopy (SERS) coupled with impedance spectroscopy. Contrary to the conventional view that surface-adsorbed sulfur is removed mainly by oxygen anions, it is found that –SO 4 groups on the surface of the proton conductor are converted to SO 2 by a water-mediated process, as confirmed by operando SERS analysis and density functional theory (DFT)-based calculations. Furthermore, the combination of operando SERS performed on a model electrode and theoretical computation offers an effective approach to investigate into complex mechanisms of electrode processes in various electrochemical systems, providing information vital to achieve the rational design of better electrode materials.

25 ENERGY STORAGE↗

The atomic geometries of GaP(110) and ZnS(110) revisited - A structural ambiguity and its resolution

The atomic geometries of GaP(110) and ZnS(110) are reexamined using the R-factor minimization procedure, developed for GaAs(110) and previously applied to GaSb(110), ZnTe(110), InAs(110), and AlP(110), to analyze experimental elastic low-energy electron diffraction intensities. Unlike most of the earlier cases, both GaP(110) and ZnS(110) exhibit two distinct minimum-Rx structures which cannot be distinguished by analysis of the shapes of the intensity profiles alone. One region of best-fit structures exhibits top-layer displacements normal to the surface characterized by a small bond-length-conserving, top-layer rotation (omega aproximately 2-3 deg), a small relaxation of the top layer away from the surface, and a 10 percent expansion of the top-layer bond length. The other region of best-fit structures is the conventional one: nearly bond-length-conserving rotations of omega = 26-28 deg in the top layer and a small (approximately 0.1 A) contraction of the uppermost layer spacing. This ambiguity may be removed, however, by consideration of the integrated beam intensities. The conventional region of structural parameters provides a decisively better description of the relative magnitudes of the integrated beam intensities and hence is the preferred structure.

Duke, C. B.↗

Identifying the Accuracy of Surface Roughness for Metal Additive Manufacturing Parts Captured with Computed Tomography Scanning

Conventional surface roughness measurement techniques require direct access to internal surfaces, often necessitating destructive sectioning of test articles. Computed tomography (CT) offers a non-destructive alternative for internal surface characterization, but its application in metrology remains unstandardized and sensitive to machine resolution and operator technique. This study investigates the feasibility of using CT scanning to quantify areal surface roughness in metal AM heat exchanger tubes with three distinct internal geometries: ribbed, discrete W, and featureless. CT-derived surface parameters were extracted using custom Python scripts and compared to measurements obtained from a focus variation microscope calibrated against a known standard. Results show that CT-based roughness measurements closely matched microscope values for the discrete W specimen, deviations between CT and microscope measurements were minimal—less than 1 µm—indicating reliable reconstruction. In contrast, the ribbed and featureless specimens, with lower roughness values showed greater discrepancies. The findings suggest that CT scanning can be a viable non-destructive metrology tool for AM parts with surface roughness above approximately 8 µm. For smoother surfaces, current CT capabilities may not provide sufficient accuracy, highlighting the need for resolution-aware workflows and further standardization in CT-based surface metrology.

36 MATERIALS SCIENCE↗

Characterization of Incremental Markings in the Sagittal Otolith of the Pacific Sardine ( Sardinops sagax ) Using Different Imaging Modalities

Teleost fish possess calcium carbonate otoliths located in separate chambers (utriculus, sacculus, and lagena) of their membranous labyrinth. This study analyzed the surface topography of the sagittal otolith of the Pacific sardine (Sardinops sagax) and the daily and annual increments in these otoliths. The otolith surface, characterized by laser scanning confocal microscopy for the first time, consisted of a system of prominent ridges and valleys (grooves), but it is unclear whether these structures are functional or represent time-resolving markings reflecting growth periodicity. Within the first-year volume, daily increments, each consisting of an incremental (more mineralized) and a discontinuous (less mineralized) zone, were resolved by optical microscopy and backscattered electron (BSE) imaging in the scanning electron microscope (SEM). Daily growth increments could, however, not be resolved in volumes formed after the first year, presumably because otolith growth markedly slows down and spacing of incremental markings narrows in older fish. Throughout otolith growth, the crystalline network continues across the discontinuous zones. Fluorochrome labeling provides additional information on growth after the first year. Compared with optical and BSE imaging, synchrotron microComputed Tomography of intact otoliths (with 0.69 µm volume elements) was less able to resolve daily increments; X-ray phase contrast reconstructions provided more detail than reconstructions with absorption contrast. Future research directions are proposed.

59 BASIC BIOLOGICAL SCIENCES↗

Surface analysis of space telescope material specimens

Qualitative and quantitative data on Space Telescope materials which were exposed to low Earth orbital atomic oxygen in a controlled experiment during the 41-G (STS-17) mission were obtained utilizing the experimental techniques of Rutherford backscattering (RBS), particle induced X-ray emission (PIXE), and ellipsometry (ELL). The techniques employed were chosen with a view towards appropriateness for the sample in question, after consultation with NASA scientific personnel who provided the material specimens. A group of eight samples and their controls selected by NASA scientists were measured before and after flight. Information reported herein include specimen surface characterization by ellipsometry techniques, a determination of the thickness of the evaporated metal specimens by RBS, and a determination of trace impurity species present on and within the surface by PIXE.

Fromhold, A. T.↗