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DOE OSTI2024

UHT-CAMANCHE: Ultra-High Temperature Ceramic Additively Manufactured Compact Heat Exchangers

The conceptual basis for this project is the convergence of advanced ultra-high temperature ceramic materials and additive manufacturing technologies to produce compact ceramic heat exchangers with complex internal flow path geometries. Task areas were broadly divided into materials and manufacturing development, heat exchanger design, component testing, and techno-economic analysis. Technical challenges included the design and commissioning of new test facilities, improving feature resolution and deposition rate of ceramic additive manufacturing techniques, establishing process-structure-property relationships in additively manufactured ultra-high temperature ceramics, and assessing high temperature materials compatibility in CO 2 environments. The primary candidate material evaluated in this work is a composite comprising zirconium diboride (ZrB2) with 30 vol. % silicon carbide (SiC) which was selected based on its desirable combination of high temperature mechanical properties, high thermal and electrical conductivities, and oxidation resistance. High solids loaded ZrB2-SiC pastes suitable for extrusion-based additive manufacturing were developed for the first time as part of this work. Materials compatibility studies indicate this material oxidizes in CO 2 to form a protective borosilicate scale which transforms to pure silica above 1000°C. Parts made by additive manufacturing displayed enlarged grain sizes produced by pressureless sintering as compared to hot-press sintering. Increases in microstructural coarseness have outsized effect on oxidation performance up to 1400°C due to incomplete oxidation of coarse large diameter SiC particles resulting in lower amounts of silica that apparently inhibit protective scale formation. Additive manufacturing as a forming technique did not appear to significantly affect thermal conductivity, hardness, or elastic modulus, though flexural strength was reduced by half or more as compared to traditionally hot-pressed materials. This effect was attributed to the presence of strength-limiting flaws (ca. 40 microns in size) originating from extrudate inhomogeneities that could potentially be eliminated with further process improvements. Attempts to attain economies of scale for production of multi-kilowatt scale heat exchangers by ceramic additive manufacturing proved difficult. Lack of automation and a modest extrusion rate while retaining fine feature resolution made the overall process labor intensive and limited experimental throughput. A number of full-scale components were taken through post-process heat treatments including drying, binder burnout, and sintering; however, none survived without significant flaws or cracks. Therefore, no operational data from a newly installed heat exchanger test loop were able to be obtained during the performance period. Continued research and development is recommended to improve economic feasibility of ceramic additive manufacturing by standardizing the use of advanced sensors, artificial intelligence, and automation tools to reduce associated labor costs and accelerate production rates. The materials and manufacturing techniques demonstrated in this work are likely to find applications in defense and energy applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Chemo‐mechanical Alterations Induced From CO 2 Injection in Carbonate‐Cemented Sandstone: An Experimental Study at 71 °C and 29 MPa

Abstract Carbon capture, utilization, and storage may lead to mechanical degradation of the subsurface reservoir from fluid‐rock interaction, which could lead to wellbore instability or reservoir compaction. To better understand potential relationship between mechanical degradation with various carbonate cement textures and compositions in sandstone reservoirs, six flow‐through experiments were conducted. Formation water (TDS = 5,390 mg/L) enriched with CO 2 flowed through two types of Pennsylvanian Morrow B Sandstone: an ankerite‐siderite‐cemented sandstone (disseminated cement texture) and a calcite‐cemented sandstone (poikilotopic cement texture). The experiments produced little change in permeability in the ankerite‐siderite‐cemented sandstone, but permeability increased up to more than 1 order of magnitude in the calcite‐cemented sandstone. Ultrasonic measurements and cylinder‐splitting tests (also known as Brazilian tests) suggested negligible mechanical degradation of the ankerite‐siderite‐cemented sandstone. Variable changes, with significant mechanical degradation in the static moduli, were observed in the calcite‐cemented sandstone. Thus, dissolution of the disseminated ankerite‐siderite cement (0.28–0.30%) had minimal impact on modifying the flow network and the mechanical integrity of the sandstone, whereas dissolution of the poikilotopic calcite cement (0.89–1.13%, quantified with fluid chemistry and visualized with X‐ray microcomputed tomography) impacted the mechanical strength of the sandstone by disconnecting framework grains. With the high water‐to‐rock mass ratios (7.3–8.2) and number of pore volumes (147–675) employed in these experiments, potential risks are most relevant to regions near injection wells. Ultimately, the chemo‐mechanical effects induced by CO 2 injection are strongly influenced by the cement texture and composition and the burial history of the reservoir rock.

Wu, Z.↗

DOE OSTI2020

Synergistic ground and orbital observations of iron oxides on Mt. Sharp and Vera Rubin ridge

Visible/short-wave infrared spectral data from the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) show absorptions attributed to hematite at Vera Rubin ridge (VRR), a topographic feature on northwest Mt. Sharp. The goals of this study are to determine why absorptions caused by ferric iron are strongly visible from orbit at VRR, and to improve interpretation of CRISM data throughout lower Mt. Sharp. These goals are achieved by analyzing coordinated CRISM and in situ spectral data along the Curiosity Mars rover’s traverse. VRR bedrock within areas that have the deepest ferric absorptions in CRISM data also have the deepest ferric absorptions measured in situ. This suggests strong ferric absorptions are visible from orbit at VRR because of the unique spectral properties of VRR bedrock. Dust and mixing with basaltic sand additionally inhibit the ability to measure ferric absorptions in bedrock stratigraphically below VRR from orbit. There are two implications of these findings: (1) Ferric absorptions in CRISM data initially dismissed as noise could be real, and ferric phases are more widespread in lower Mt. Sharp than previously reported, (2) Patches with the deepest ferric absorptions in CRISM data are, like VRR, reflective of deeper absorptions in the bedrock. One model to explain this spectral variability is late-stage diagenetic fluids that changed the grain size of ferric phases, deepening absorptions. Curiosity’s experience highlights the strengths of using CRISM data for spectral absorptions and associated mineral detections, and the caveats in using these data for geologic interpretations and strategic path planning tools.

58 GEOSCIENCES↗

DOE OSTI2022

High-Silicon Steel Strip by Single-Step Shear Deformation Processing

It is well known that Fe-Si alloys with Si content higher than in conventional electrical sheet steels (>3.2% Si) can make a significant impact in improving the efficiency of electrical motors if they are available in sheet/foil (strip) forms at suitable cost. While the magnetic and electrical attributes (e.g., resistivity, core loss) of these high-Si Fe alloys, of relevance to electrical motor core laminations, are known to be exceptional, the alloys have limited workability, making them difficult to produce consistently in sheet/foil (strip) forms. Current processing techniques such as rolling, while adequate for producing conventional electrical steel sheet, do have important disadvantages - large energy consumption and emissions, limitations in processing of low-workability alloys (e.g., high-Si content steels), large-scale plant infrastructure, and less than adequate capability to engineer sheet metals with specific microstructures (e.g., fine-grained) and crystallographic textures (e.g., shear textures). It is therefore of interest to have an alternative commercial process that can produce sheet/foil (strip) from high-Si Fe alloys and which can also overcome some of the deficiencies of current multistage strip processes. The goal of the present project was design and demonstration of a new energy-efficient pilot process for producing high-Si electrical steel strip of commercial widths and thickness, and with superior electrical and magnetic properties than current electrical steels (Fe-3.2% Si as benchmark). The applications domain for these steels is electrical motor core laminations. We have addressed this goal by accomplishment of the following specific objectives and tasks: a) Development of an Fe-4Si-4Cr alloy with electrical resistivity >80 μΩ-cm, induction flux density >1.48 T at 5000 A/m and core loss 35% lower than the benchmark 3.2% Si alloy. The alloy which meets DOE target specifications for motor core attributes was designed with the Si content controlled for the electrical properties and the Cr content tailored to meet material/process workability requirements. b) A unique machining-based deformation processing system was designed and scaled-up to produce strip of commercial width (25 mm to 150 mm) and thickness (up to 0.5 mm) from the Fe-4Si-4Cr alloy and other alloys of varied workability including copper, Al6061-T6 and naval brass. The key attributes of the machining-based strip production are deformation processing by concentrated simple-shear; single-step production of strip from ingot using compact machine infrastructure; strip surface finish of Ra 0.35 to 1 micrometer that is comparable/superior to that of rolled strip; discrete production of strip that can potentially be done at point of use; and controllability of strip mechanical/formability properties by deformation control. c) The electrical, magnetic, surface quality, mechanical, formability, and metallurgical properties/attributes of the machining-based strip were established by direct ASTM standard or equivalent measurement techniques. d) Punching characteristics of the strip in terms of load, edge quality and macro defects were similar to those of conventional 3.2% Si electrical steels. These punching characteristics are critical from a manufacturability perspective for motor/transformer core applications. e) A modeling framework for energy analysis of multistage rolling and the machining-based deformation processing has been established. Application of this modeling to the two strip-processes showed that the machining-based process requires significantly lower specific energy for processing, ~ 25% of that for rolling. The modeling framework can be adapted for a range of sheet-metal forming, bulk metal forming, and machining processes. It can be used to identify key parameters controlling process specific energy. f) A comparative analysis of advantages and disadvantages of machining-based processing against rolling for strip production. The single stage machining-based processing, with compact infrastructure, represents a new manufacturing paradigm for sheet and foil manufacturing that can potentially also be applied to advanced titanium, aluminum, copper and magnesium alloys. The goals and objectives were accomplished by a cross-disciplinary project team comprising of personnel from Purdue University; M4 Sciences LLC, a small-business focused on advanced manufacturing technology development; the Pacific Northwest National Labs; and tool manufacturers. The team is currently in advanced discussions with multiple entities for future process development for commercialization.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Physical properties, internal structure, and the three‐dimensional petrography of CI chondrites

physical properties and the nature of their breccation, we investigated nine samples of the Ivuna and Orgueil CI chondrites ranging in size from 1 mm to 4 cm in approximate diameter. The combined mass of unique material investigated in this work is 113 g. For our investigations, we use ideal gas pycnometry, 3-D laser scanning, x-ray computed microtomography (μCT), and accompanying digital data extraction techniques. We found that the bulk density of the samples ranged from 1.61 to 2.10 g cm −3 . Larger samples tend to have a lower bulk density. Grain density (ranging from 2.44 to 2.55 g cm −3 ) is significantly less variable than the bulk density in our samples and the quantity of porosity (ranging from 14.6% to 33.8%) is the dominant factor in determining the bulk density of CI chondrite material. Our μCT results show that the visible porosity across all sizes of our CI chondrite samples is in the form of cracks, but these cracks can account for less than two-thirds of the porosity in the CI chondrites. Other porosity is not visible, even at μCT resolutions of 2.7 μm voxel edge −1 and we conclude that it is sub-micron in nature. It is not clear if the cracks seen in our samples are indigenous to the chondrites or are a result of terrestrial processes. We also find that the CI chondrites are excellent examples of the fractal-like nature of brecciation, where clasts can be observed at all scales we imaged. The breccias are composed of sub-equant-shaped and sub-rounded-textured clasts like melt-free impact breccias on other solar system bodies. From our μCT volume and digital data extraction, we determine that the Ivuna CI chondrite breccia is organized: the mostly sub-equant clasts within our ~2 cm chunk of Ivuna have a mean diameter of 1.33 mm and their aligned longest axes define a lineation structure. We speculate that the lineation was imparted after fragmentation of the clasts by slight shear on the parent asteroid which could be the result of seismic-related granular flow or mild non-axial impact-related compaction. These data will help to place returned asteroidal material from asteroids 162173 Ryugu and 101955 Bennu and the CI chondrites into a mutual geological context.

CI chondrite↗