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All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Utilization of the St. Peter Sandstone in the Illinois Basin for CO2 Sequestration

This project is part of a larger project co-funded by the United States Department of Energy (US DOE) under cooperative agreement DE-FE0002068 from 12/08/2009 through 9/31/2014. The study is to evaluate the potential of formations within the Cambro-Ordovician strata above the Mt. Simon Sandstone as potential targets for carbon dioxide (CO2) sequestration in the Illinois and Michigan Basins. This report evaluates the potential injectivity of the Ordovician St. Peter Sandstone. The evaluation of this formation was accomplished using wireline data, core data, pressure data, and seismic data acquired through funding in this project as well as existing data from two additional, separately funded projects: the US DOE funded Illinois Basin – Decatur Project (IBDP) being conducted by the Midwest Geological Sequestration Consortium (MGSC) in Macon County, Illinois, and the Illinois Industrial Carbon Capture and Sequestration (ICCS) Project funded through the American Recovery and Reinvestment Act (ARRA), which received a phase two award from DOE. This study addresses the question of whether or not the St. Peter Sandstone may serve as a suitable target for CO2 sequestration at locations within the Illinois Basin where it lies at greater depths (below the underground source of drinking water (USDW)) than at the IBDP site. The work performed included numerous improvements to the existing St. Peter reservoir model created in 2010. Model size and spatial resolution were increased resulting in a 3 fold increase in the number of model cells. Seismic data was utilized to inform spatial porosity distribution and an extensive core database was used to develop porosity-permeability relationships. The analysis involved a Base Model representative of the St. Peter at “in-situ” conditions, followed by the creation of two hypothetical models at in-situ + 1,000 feet (ft.) (300 m) and in-situ + 2,000 ft. (600 m) depths through systematic depthdependent adjustment of the Base Model parameters. Properties for the depth shifted models were based on porosity versus depth relationship extracted from the core database followed by application of the porosity-permeability relationship. Each of the three resulting models were used as input to dynamic simulations with the single well injection target of 3.2 million tons per annum (MTPA) for 30 years using an appropriate fracture gradient based bottom hole pressure limit for each injection level. Modeling results are presented in terms of well bottomhole pressure (BHP), injection rate profiles, and three-dimensional (3D) saturation and differential pressure volumes at selected simulation times. Results suggest that the target CO2 injection rate of 3.2 MTPA may be achieved in the St. Peter Sandstone at in-situ conditions and at the in-situ +1,000 ft. (300 m) depth using a single injector well. In the latter case the target injection rate is achieved after a ramp up period which is caused by multi-phase flow effects and thus subject to increased modeling uncertainty. Results confirm that the target rate may not be achieved at the in-situ +2,000 ft. (600 m) level even with multiple wells. These new modeling results for the in-situ case are more optimistic than previous modeling results. This difference is attributed to the difference in methods and data used to develop model permeability distributions. Recommendations for further work include restriction of modeling activity to the in-situ +1,000 ft. (300 m) and shallower depth interval, sensitivity and uncertainty analysis, and refinement of porosity and permeability estimates through depth and area selective querying of the available core database. It is also suggested that further modeling efforts include scope for evaluating project performance in terms of metrics directly related to the Environmental Protection Agency (EPA) Class VI permit requirements for the area of review (AoR) definition and post injection site closure monitoring.

Will, Robert↗
DOE OSTI2014

The Potosi Reservoir Model 2013c, Property Modeling Update

As part of a larger project co-funded by the United States Department of Energy (US DOE) to evaluate the potential of formations within the Cambro-Ordovician strata above the Mt. Simon as potential targets for carbon sequestration in the Illinois and Michigan Basins, the Illinois Clean Coal Institute (ICCI) requested Schlumberger to evaluate the potential injectivity and carbon dioxide (CO2) plume size of the Cambrian Potosi Formation. The evaluation of this formation was accomplished using wireline data, core data, pressure data, and seismic data from this project as well as two other separately funded projects: the US DOE-funded Illinois Basin–Decatur Project (IBDP) being conducted by the Midwest Geological Sequestration Consortium (MGSC) in Macon County, Illinois, and the Illinois Industrial Carbon Capture and Sequestration (ICCS) project funded through the American Recovery and Reinvestment Act. In 2010, technical performance evaluations on the Cambrian Potosi Formation were performed through reservoir modeling. The data included formation tops from mud logs, well logs from the Verification Well #1 (VW1) and the Injection Well (CCS1), structural and stratigraphic formation from three dimensional (3D) seismic data, and field data from several waste water injection wells for Potosi Formation. The intention was for 2.2 million tons per annum (2 million tonnes per annum [MTPA]) of CO2 to be injected for 20 years. In the Task Error! Reference source not found., the 2010 Potosi heterogeneous model (referred to as the "Potosi Dynamic Model 2010") was re-run using a new injection scenario of 3.5 million tons per annum (3.2 MTPA) for 30 years. The extent of the Potosi Dynamic Model 2010, however, appeared too small for the new injection target. The models size was insufficient to accommodate the evolution of the plume. The new model, Potosi Dynamic Model 2013a, was built by extending the Potosi Dynamic Model 2010 grid to 30 by 30 mi (48 by 48 km), while preserving all property modeling workflows and layering. This model was retained as the base case. In the preceding Task [1], the Potosi reservoir model was updated to take into account the new data from the Verification Well #2 (VW2) which was drilled in 2012. The porosity and permeability modeling was revised to take into account the log data from the new well. Revisions of the 2010 modeling assumptions were also done on relative permeability, capillary pressures, formation water salinity, and the maximum allowable well bottomhole pressure. Dynamic simulations were run using the injection target of 3.5 million tons per annum (3.2 MTPA) for 30 years. This dynamic model was named Potosi Dynamic Model 2013b. In this Task, a new property modeling workflow was applied, where seismic inversion data guided the porosity mapping and geobody extraction. The static reservoir model was fully guided by PorosityCube interpretations and derivations coupled with petrophysical logs from three wells. The two main assumptions are: porosity features in the PorosityCube that correlate with lost circulation zones represent vugular zones, and that these vugular zones are laterally continuous. Extrapolation was done carefully to populate the vugular facies and their corresponding properties outside the seismic footprint up to the boundary of the 30 by 30 mi (48 by 48 km) model. Dynamic simulations were also run using the injection target of 3.5 million tons per annum (3.2 MTPA) for 30 years. This new dynamic model was named Potosi Dynamic Model 2013c. Reservoir simulation with the latest model gives a cumulative injection of 43 million tons (39 MT) in 30 years with a single well, which corresponds to 40% of the injection target. The injection rate is approx. 3.2 MTPA in the first six months as the well is injecting into the surrounding vugs, and declines rapidly to 1.8 million tons per annum (1.6 MTPA) in year 3 once the surrounding vugs are full and the CO2 start to reach the matrix. After, the injection rate declines gradually to 1.2 million tons per annum (1.1 MTPA) in year 18 and stays constant. This implies that a minimum of three (3) wells could be required in the Potosi to reach the injection target. The injectivity evaluated in this Task was higher compared to the preceding Task, since the current facies modeling (guided by the porosity map from the seismic inversion) indicated a higher density of vugs within the vugular zones. 5 As the CO2 follows the paths where vugs interconnection exists, a reasonably large and irregular plume extent was created. After 30 years of injection, the plume extends 13.7 mi (22 km) in E-W and 9.7 mi (16 km) in N-S directions. After injection finishes, the plume continues to migrate laterally, mainly driven by the remaining pressure gradient. After 60 years post-injection, the plume extends 14.2 mi (22.8 km) in E-W and 10 mi (16 km) in N-S directions, and remains constant as the remaining pressure gradient has become very low. Should the targeted cumulative injection of 106 million tons (96 MT) be achieved; a much larger plume extent could be expected. The increase of reservoir pressure at the end of injection is approximately 1,200 psia (8,274 kPa) around the injector and gradually decreases away from the well. The reservoir pressure increase is less than 10 psia (69 kPa) beyond 14 mi (23 km) away from injector. Should the targeted cumulative injection of 106 million tons (96 MT) be achieved; a much larger areal pressure increase could be expected. The reservoir pressure declines rapidly during the first 30 years post injection and the initial reservoir pressure is nearly restored after 100 years post-injection. The present evaluation is mainly associated with uncertainty on the vugs permeability and interconnectivity. The use of porosity mapping from seismic inversion might have reduced the uncertainty on the lateral vugs body distributions. However, major uncertainties on the Potosi vugs permeability remains. Therefore, injection test and pressure interference test among the wells could be considered to evaluate the local vugs permeability, extent, and interconnectivity. Facies modeling within the Potosi has yet to be thoroughly addressed. The carbonates during the time of deposition are believed to be regionally extensive. However, it may be worth delineating the reservoir with other regional wells or modern day analogues to understand the extent of the Potosi. More specifically, the model could incorporate lateral changes or trends if deemed necessary to represent facies transition. Data acquisitions to characterize the fracture pressure gradient, the formation water properties, the relative permeability, and the capillary pressure could also be considered in order to allow a more rigorous evaluation of the Potosi storage performance. A simulation using several injectors could also be considered to determine the required number of wells and appropriate spacing to achieve the injection target while taking into account the pressure interference.

Adushita, Yasmin↗
DOE OSTI2019

Multivariate Analysis of the Influence of Process Parameters on Suspension Plasma-Sprayed Coatings

Suspension plasma spray (SPS) is far more complicated than conventional plasma spray and requires a deep knowledge about the influence of process parameters and their correlations. In this study, YSZ coatings were manufactured by SPS with six different process parameters such as plasma power, suspension mass load, original powder size, substrate surface topology, spray distance, and spray step. Afterwards, the porosity of as-prepared coatings was investigated by image method and X-ray transmission technique. A multivariate analysis on the collected experimental data was carried out by employing mathematical statistics methods. The results showed that: 1) Coating porosity has a negative correlation with plasma power and suspension mass load and a positive correlation with the original powder size, spray distance, spray step, and substrate roughness; 2) Spraying distance is the main factor affecting to coating porosity, followed by suspension mass load and substrate surface roughness, respectively. A linear model for porosity prediction was developed and was verified by experiments. The mechanism by which process parameters influence coating porosity is also discussed.

Zhao, Yongli↗
DOE OSTI2022

Hierarchical printed product and composition and method for making the same

Disclosed herein are embodiments of a printable composition that can be used to make printed products of a chosen material chemistry that have different levels of porosity within the printed product's structure Also disclosed herein are embodiments of a printed product that has multiple levels of porosity throughout its structure, which can include a macroscale level of porosity, a microscale level of porosity, a nanoscale level of porosity and any combination thereof. These printed products can be made using a 3-D printer and can be made from a single printable composition without the need to add different structural components during the production process. Also disclosed herein are embodiments of a method for making and using a printed product.

Lee, Matthew N.↗
DOE OSTI2025

Reaction-Induced Fracturing of Porous Carbonate Rocks during Volume-Increasing Replacement by Witherite

Volume-increasing replacement reactions can lead either to fracturing of the parent phase or to the formation of cohesive layers that passivate further reaction, but the factors that drive one outcome or the other are not understood. In this experimental study, we investigated the volume-increasing replacement of carbonate rocks (consisting of CaCO 3 and CaMg(CO 3 ) 2 ) of different porosity by witherite (BaCO 3 ). Samples were characterized using scanning electron microscopy, Raman spectroscopy, small-angle neutron/X-ray scattering, X-ray tomography, and scanning transmission electron microscopy. We observed the formation of a witherite reaction layer and witherite formation within pores and along grain boundaries. Despite this being a volume-increasing replacement reaction, newly formed witherite was porous, potentially allowing further replacement. Filled fractures were observed in the low-porosity carbonates, whereas witherite formed within pores in high-porosity carbonates. We conclude that fracturing of the parent phase versus passivation is contingent on the initial microstructure of the parent with an optimal degree of porosity required for fracturing.

Calcite↗
DOE OSTI2015

Mechanism of formation of wiggly compaction bands in porous sandstone: 1. Observations and conceptual model

Field observations are combined with microscopic analyses to investigate the mechanism of formation of wiggly compaction bands (CBs) in the porous Jurassic aeolian Aztec Sandstone exposed at Valley of Fire State Park, Nevada. Among the three types of CBs (T1, T2, and T3), we focused on the wiggly CBs (T3), which show a chevron (T3 1 ) or wavy (T3 2 ) pattern with typical corner angles of approximately 90° or 130°, respectively. Where corner angles of wiggly CBs increase to 180°, they become straight CBs (T3 3 ). Image analyses of thin sections using an optical microscope show host rock porosity increases downslope in this dune, and the predominant type of wiggly CBs also varies from chevron to straight CBs. Specifically, band type varies continuously from chevron to wavy to straight where the porosity and grain sorting of the host rock increase systematically. Based on the crack and anticrack models, we infer that the change from chevron to straight CBs is due to increasing failure angle of the sandstone and this may correlate with increasing grain sorting. Wavy CBs with intermediate failure angle and host rock porosity are an intermediate stage between chevron and straight CBs. Previous sedimentological studies also have suggested that grain size and sorting degree increase downslope on the downwind side of sand dunes due to a sieving process of the wind-blown grains. Furthermore, the transition of wiggly CB types in this regard correlates with increasing sorting and perhaps with increasing porosity downslope.

58 GEOSCIENCES↗
DOE OSTI2017

Fracture capture of organic pores in shales

Shales are heterogeneous media with porosity at many scales and in many microtextural positions, including within organic matter and clay aggregates. Because these materials have contrasting mechanical properties, it remains unclear how induced fractures manage to connect with this porosity whether during hydrocarbon production, wastewater injection, or carbon-capture-and-storage efforts. To explore porosity changes related to fracturing, we experimentally failed shale samples in a triaxial load apparatus and observed changes in microstructure through scanning electron microscopy, low-pressure nitrogen sorption, and nuclear magnetic resonance. We observed a system of microcracks, many of which were likely experimentally induced and localized on grain boundaries. In some cases these fractures propagated into regions of natural porosity in organic matter. In the subsurface this “fracture capture” likely enhances pore connectivity, but only selectively depending upon mechanical conditions. Finally, fracture capture is one possible mechanism by which multiscale compositional heterogeneity in shales may affect rheological heterogeneity.

58 GEOSCIENCES↗
DOE OSTI2026

Optimization of Processing, Microstructure, and Hardness of an Al–Ce–Ni–Mn–Zr Alloy With Laser Additive Manufacturing

Here, this study examines the processing behavior, microstructure, surface roughness, and hardness properties of an aluminum alloy containing 8.2 Ce, 4.5 Ni, 0.5 Mn, and 0.7 Zr (wt%) fabricated using laser powder bed fusion. Sixty samples were produced across a range of laser powers, scan speeds, and hatch spacings to evaluate their effect on porosity, hardness, and microstructural features. Porosity was measured using X-ray computed tomography, while microstructure and surface roughness were characterized by scanning electron (SEM) and laser confocal microscopy. High dense and cracking-free Al–Ni–Ce alloy was successfully manufactured. Porosity showed a U-shaped dependence on energy input, increasing under both insufficient and excessive melting conditions. Hardness increased with cooling rate due to finer cellular structures and solute redistribution. A general statistical model was developed to capture the relationships between processing parameters and material response. Results identify a narrow processing window defined by laser powers between 350 and 370 W, scan speeds from 1400 to 1800 mm/s, and hatch distances between 0.14 and 0.18 mm. Within this window, porosity is minimized (below 0.01%) and hardness is maximized (up to 160 HV), demonstrating that careful control of these parameters enables dense, high strength aluminum components suitable for demanding structural applications.

Aluminum alloys↗
DOE OSTI2025

Isolated vesicles in submarine pumice: insights from the 2019 Volcano F eruption, Kingdom of Tonga

No reliable method can distinguish between subaerial and submarine pumice, but recent work shows that highly vesicular (total porosity, φ > 65%) submarine pumice from the 2012 Havre and 2021 Fukutoku Oka-no-Ba eruptions contains abundant isolated porosity (connectivity, C < 0.6). This differs from textural measurements of subaerial pumice with similarly high vesicularities, where high connectivities (C > 0.8) are often measured. To investigate the implications of this under-studied texture for bubble nucleation, growth, and coalescence dynamics at submarine eruptions, we analyze the textural characteristics of rafted pumice clasts from the 2019 submarine eruption of Volcano F, located along the Tonga-Kermadec Arc. We examined clasts collected while floating near the vent (50–200 km) and distally on the shores of Fiji (900 km). Using helium pycnometry and X-ray tomography (XRT), we quantified porosity and connectivity in 45 pumice lapilli, classifying them by vesicle macrotexture and edge morphology. Microvesicular clasts, the majority of which have breadcrust and cauliflower textures, exhibit the lowest connectivities (C = 0.61 ± 0.2), while macrovesicular clasts have high connectivities with C ~ 1. We propose that isolated porosity abundance varies according to clast location in the eruption column post-fragmentation. Microvesicular clasts erupted on the edges of the column and experienced high levels of seawater ingestion and subsequent quenching of the entire clast. Macrovesicular clasts, in contrast, erupted in the center of the eruption column and were thus thermally insulated, allowing magmatic bubbles in the molten pumice to nucleate, grow, and coalesce for longer. Our results and interpretation imply that low connectivity, microvesicular clasts preserve pre and syn-eruptive bubble processes at the 2019 Volcano F eruption.

Permeability↗
DOE OSTI2019

Predicting the reliability of an additively-manufactured metal part for the third Sandia fracture challenge by accounting for random material defects

We describe an approach to predict failure in a complex, additively-manufactured stainless steel part as defined by the third Sandia Fracture Challenge. A viscoplastic internal state variable constitutive model was calibrated to fit experimental tension curves in order to capture plasticity, necking, and damage evolution leading to failure. Defects such as gas porosity and lack of fusion voids were represented by overlaying a synthetic porosity distribution onto the finite element mesh and computing the elementwise ratio between pore volume and element volume to initialize the damage internal state variables. These void volume fraction values were then used in a damage formulation accounting for growth of these existing voids, while new voids were allowed to nucleate based on a nucleation rule. Blind predictions of failure are compared to experimental results. The comparisons indicate that crack initiation and propagation were correctly predicted, and that an initial porosity field superimposed as higher initial damage may provide a path forward for capturing material strength uncertainty. Here, the latter conclusion was supported by predicted crack face tortuosity beyond the usual mesh sensitivity and variability in predicted strain to failure; however, it bears further inquiry and a more conclusive result is pending compressive testing of challenge-built coupons to de-convolute materials behavior from the geometric influence of significant porosity.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Geohydrodynamic Parameters and Their Implications on the Coastal Conservation: A Case Study of Abak Local Government Area (LGA), Akwa Ibom State, Southern Nigeria

A total of 14 vertical electrical soundings using Schlumberger electrode configuration and the complementary laboratory analysis of aquifer samples were carried out in the Abak Local Government Area of Akwa Ibom State, the coastal region of Nigeria. The study focused on the estimation of geohydrodynamic parameters of the frequently exploited aquifers and the implication of hydrodynamic parameters on the lithostratigraphy and the anticipated exposure of the assessed geologic formation at the shorelines. These parameters were porosity (&straightphi;), tortuosity (τ), formation factor (F), aquifer water formation resistivity (R{sub w}) and coefficient of permeability/hydraulic conductivity (K). Computation of the effective porosities from the aquifer cuttings was carried out using wet weight–dry weight technique and petrophysical techniques. The F values were computed using the aquifer formation bulk resistivity measured from field 1-D resistivity data analysis, whose interpretation was constrained by nearby borehole information. The formation pore water resistivities were estimated from the laboratory using electrical resistivity metre. The Win RESIST software program was used in interpreting the field data electronically. The results of interpretation gave the primary parameters of saturated and unsaturated units of the coastal regions used in this work. The area generally shows seemingly high porosity with high coefficient of permeability. The primary and secondary parameters have been contoured to model their distributions. Besides, some functional relations have been realized through regression analyses. The contour distribution of the geohydrodynamic parameters indicates the vulnerability of the water repositories to contaminations as well as the vulnerability of the shoreline to waterborne erosion. The seemingly high effective porosity in the compliant laboratory and calculated values indicate that the coastal region is neither lithified nor compacted/consolidated. This signals the possibility of the formation to be easily eroded, weathered or flooded where these units are exposed to water current. With these revelations, the shorelines could be properly managed and conserved by geotechnically reinforcing with hard and water-resistant concrete that can protect the vulnerable and erosion-prone porous sediments.

58 GEOSCIENCES↗
DOE OSTI2018

Effect of Pore Size, Morphology and Orientation on the Bulk Stiffness of a Porous Ti35Nb4Sn Alloy

The metal foams of a titanium alloy were designed to study porosity as well as pore size and shape independently. These were manufactured using a powder metallurgy/space-holder technique that allowed a fine control of the pore size and morphology; and then characterized and tested against well-established models to predict a relationship between porosity, pore size and shape, and bulk stiffness. Among the typically used correlations, existing power-law models were found to be the best fit for the prediction of macropore morphology against compressive elastic moduli, outperforming other models such as exponential, polynomial or binomial. Other traditional models such as linear ones required of updated coefficients to become relevant to metal porous sintered macrostructures. The new coefficients reported in this study contribute toward a design tool that allows the tailoring of mechanical properties through porosity macrostructure. The results show that, for the same porosity range, pore shape and orientation have a significant effect on mechanical performance and that they can be predicted. Conversely, pore size has only a mild impact on bulk stiffness.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Fabrication and Characterization of Core–Shell Density-Graded 316L Stainless Steel Porous Structure

In the present work, cylindrical shape 316 L cellular structure with different densities in its core and outer layer (shell) is fabricated by using carbamide as a space holder, via powder metallurgy route and layer-by-layer technique. The arrangement of the created pore is the same as face-centered cubic atomic structure, and different densities are created in two regions by using carbamide particles having two different sizes in the range of 1.7-2 and 2-2.4 mm. The effect of creating a structure with higher porosity (64.5%) in the core and lower porosity (53.8%) in the shell and vice versa and also change in the ratio of the core to the cylinder cross-sectional areas, on the mechanical properties and compaction load bearing of the fabricated foam samples were investigated. In leaching process of the carbamide particles, as an important step of porous structure’s fabrication, it is shown that discontinuous leaching process is more favorable than continuous, by which it would be possible to remove more carbamide particles (around 20%) at the same time. Furthermore, the deformation of the density-graded foam shows the parallel mechanism in the core and shell sections, and the contribution of each part depends on its density and thickness. The energy absorption behavior of the fabricated specimens is evaluated optimally in terms of the energy absorption value associated with the ideal adsorption behavior. The maximum ideal energy absorption efficiency for the samples with more porosity in the shell was approximately equal to 0.91, while for the sample includes the lower amount of porosity in the shell, this value was in the range of 0.85 and 0.89.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Annealing on the Impact Resistance and Fracture Mechanism of PNC-60 Sinters After Cold Plastic Deformation

Compaction of sintered metal powders by free upsetting at room temperature dangerously reduces their plastic properties, particularly the fracture toughness. The reason for the occurrence of two unfavorable phenomena accompanying this deformation route is sought. The first phenomenon depends on the initial porosity of the preform and the amount of cold work resulting in the destruction of bonds and violation of continuity between sintered powder particles. The second phenomenon is the deformation of the metal matrix, which reduces the plasticity of the sintered product. To correctly assess the effect of changes occurring in the matrix as a result of deformation, it is necessary to use the properly defined sintered matrix hardening parameter discussed in this study. The adverse effects of cold forming can be eliminated by annealing the deformed sinters at a temperature below the sintering point and above the recrystallization temperature. The annealing temperature causes favorable changes in the structure and increases the impact resistance of the deformed sinters depending on the degree of deformation of the sintered matrix and the initial porosity of the preform. Annealing at a properly selected temperature restores the ductility of the metal matrix and improves the integrity of the sintered material impaired by the effect of deformation. Annealing also causes favorable changes in the porosity morphology, removing defects in the form of gaps and resulting in the spheroidization of voids. With an appropriately selected initial porosity and degree of deformation, subsequent annealing of sinters compacted by free cold upsetting provides products with strength properties comparable to sinters with the same density and subjected to single compaction and sintering but with considerably higher fracture toughness.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effect of microstructure and temperature on nuclear graphite oxidation using the 3D Random Pore Model

This work compared the 3D Random Pore Model (3D-RPM) with experimental and characterization data to systematically study the effect of nuclear graphite microstructure and air oxidation temperature. It is well known that oxidation-induced weight loss at elevated temperatures degrades graphite structure and properties; however, a fundamental understanding of the role of graphite microstructure is still unclear. In this work, three diverse grades of nuclear graphite—IG-110, NBG-18, and PCEA—were examined and tested at air oxidation temperatures of 600, 650, 700, and 750 °C following ASTM D7542. Here, the 3D-RPM reproduced the microstructure and temperature dependence of mass loss curves for these grades. For the first time, measurements and modeling were combined to show how bulk density and the amount and spatial distribution of open and closed porosity affects oxidation. IG-110 was less dense and had an open pore network that is finer and more uniformly spread, and showed fastest oxidation. PCEA porosity was less uniform and showed less oxidation, while NBG-18 was more dense, had the least fine and uniform porosity, and showed the slowest oxidation. In general, oxidation proceeds faster if open porosity is more uniformly distributed and can incrementally access closed pore surface area with more ease.

36 MATERIALS SCIENCE↗
DOE OSTI2012

X-ray microtomography shows pore structure and tortuosity in alkali-activated binders

Durability of alkali-activated binders is of vital importance in their commercial application, and depends strongly on microstructure and pore network characteristics. X-ray microtomography ({mu}CT) offers, for the first time, direct insight into microstructural and pore structure characteristics in three dimensions. Here, {mu}CT is performed on a set of sodium metasilicate-activated fly ash/slag blends, using a synchrotron beamline instrument. Segmentation of the samples into pore and solid regions is then conducted, and pore tortuosity is calculated by a random walker method. Segmented porosity and diffusion tortuosity are correlated, and vary as a function of slag content (slag addition reduces porosity and increases tortuosity), and sample age (extended curing gives lower porosity and higher tortuosity). This is particularly notable for samples with {>=} 50% slag content, where a space-filling calcium (alumino)silicate hydrate gel provides porosity reductions which are not observed for the sodium aluminosilicate ('geopolymer') gels which do not chemically bind water of hydration.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of the hydration temperature on the microstructure of Class G cement: C-S-H composition and density

Curing temperature has a significant influence on cement paste microstructure and the properties of its principal hydrate C-S-H. In this paper, the effect of the hydration temperature in the range of 7 °C to 90 °C on the microstructure of a class G oil-well cement is studied. This is done by combining various experimental methods, including X-ray diffraction associated with the Rietveld analysis, thermo-gravimetric analysis, mercury intrusion porosimetry and porosity evaluation by drying. The experimental results show an increase of the capillary porosity and a decrease of the gel porosity by increasing the hydration temperature. This is attributed to a decrease of the C-S-H intrinsic porosity and a corresponding increase of the C-S-H density for higher curing temperatures. The experimental results are used in a simple analysis method to evaluate the density of C-S-H, as well as its C/S ratio and H/S ratio in dry and saturated conditions. The evaluated C-S-H density varies from 1.88 g/cm{sup 3} at 7 °C to 2.10 g/cm{sup 3} at 90 °C. The results also show a decrease of molar C/S ratio with increasing hydration temperature from 1.93 at 7 °C to 1.71 at 90 °C and of the H/S ratio from 5.1 at 7 °C to 2.66 at 90 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of the hydration temperature on the pore structure of cement paste: Experimental investigation and micromechanical modelling

The hydration temperature has a considerable effect on the microstructure of cement paste. The microstructural changes with increasing curing temperature result in a significant decrease of cement mechanical properties. The present work aims at studying these phenomena via micromechanical modelling, based on an experimental characterization of cement microstructure. The pore structure of a class G oil-well cement paste (American Petroleum Institute classification) hydrated at different temperatures, between 7 °C and 90 °C is characterized. Then, the influence of the microstructure variations on the elastic properties of the hardened paste is explored through micromechanical modelling. A previous analysis of the microstructure enabled determining the volume fractions of different phases of a class G cement paste hydrated under different temperatures [1]. A multiscale self-consistent homogenization model is used based on these results to simulate the variations of the mechanical properties with hydration temperature. The results are compared with macro-scale elastic properties obtained from uniaxial compression tests. It is shown that the increasing capillary porosity with elevating hydration temperature, is not sufficient to fully explain this drop of elastic properties. The latter originates mainly from the decrease of the elastic properties of the foam composed of the porous C-S-H intermixed with capillary pores. The pore structure analysis coupled with the micromechanical modelling permitted a back-analysis of the intrinsic porosities of high density and low density C-S-H showing an almost constant LD intrinsic porosity and a significantly decreasing HD intrinsic porosity.

36 MATERIALS SCIENCE↗