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At least 721 records · Page 40
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Facile, low-energy routes for the production of hydrated calcium and magnesium salts from alkaline industrial wastes

Divalent ions are extracted from solids by leaching to form a divalent ion-containing solution. The divalent ion-containing solution is subjected to concentration to form a concentrated divalent ion-containing solution. Precipitation of a divalent ion hydroxide salt is induced from the concentrated divalent ion-containing solution. In other cases, the concentrated divalent ion-containing solution is exposed to carbon dioxide to induce precipitation of a divalent ion carbonate salt.

Sant, Gaurav N.↗
DOE OSTI2023

Salt hydrate-based phase change thermal energy storage and encapsulation thereof

Among other things, the present disclosure relates to phase change material (PCM) composites composed of an PCM mixed with a nucleating agent contained within the pores of a graphite matrix and/or a hydrogel. The process to create these PCM composites includes coating the surface of graphite with a surfactant, compressing the graphite to form a matrix, then filling the graphite matrix with the PCM.

Odukomaiya, Adewale↗
DOE OSTI2023

Direct observation of C 3 S particle dissolution using fast nano X-ray computed tomography

Tricalcium silicate (C 3 S) occupies 50 % to 70 % of ordinary portland cement (OPC) by mass and it is an important component affecting the hydration of OPC [1], [2], [3], [4], [5], [6], [7]. Generally, the hydration of C 3 S is described by two processes: the dissolution of C 3 S particles and the precipitation of hydration products. While it is understood that the dissolution rates of C 3 S vary with time, more precise measurements are needed to understand this process. Many mechanisms have been proposed to explain the time-evolving dissolution rates of C 3 S [2]. The metastable barrier hypothesis suggests that a thin metastable layer of hydrates forms around the C 3 S particle surface and prohibits the access of grains to the aqueous solution [8], [9], [10], [11], [12]. The slow dissolution step hypothesis suggests that the increased ion concentration from the initial reaction delays the C 3 S dissolution [2], [13], [14], [15], [16], [17]. More recent publications suggest that C 3 S may react differently depending on the existence of crystallographic defects [18], [19], [20]. Etch pits are thought to open on the particle surface during the initial reaction and this contributes to the C 3 S dissolution [21], [22]. As hydrates precipitate and cover these highly reactive surfaces, hydration slows down and the induction period starts [18], [23], [24], [25], [26]. Many experiments have been conducted to test the aforementioned mechanisms. Some hydration studies utilize bulk measurements, such as isothermal calorimetry [27], [28], [29], pore solution analysis [30], quasi-elastic neutron scattering [31], and nuclear magnetic resonance spectroscopy [32], [33]. One limitation of these measurements is that they do not provide direct and detailed information on the individual C 3 S particles. Some other studies utilize imaging techniques, such as scanning electron microscopy (SEM) [34], [35], [36] and transmission electron microscopy (TEM) [37]. However, SEM/TEM cannot track the evolution of individual particles throughout hydration [34], [35], [38], [39], [40] and they do not give insights into the microstructure of materials before hydration [34], [35], [39]. This makes it challenging to draw strong conclusions from only SEM or TEM observations. Synchrotron X-ray tomography techniques have been used more broadly in recent years to study cement hydration. They are not only non-destructive but also able to image a sample in full 3D with resolutions that can reach from micron to nanoscale. Nano computed tomography (nCT) is one technique that has been applied to study cement hydration at the nanoscale [26], [41]. A typical nCT can reach a pixel size from 15 to 65 nm, providing enough detail for observing features <1 μm. However, nCT often takes >0.5 h to finish one scan. This makes the application of this technique on continuous scans for in-situ observations challenging. Fast X-ray computerized tomography (fCT) is another technique that has shown success in studying the time-evolving cement microstructures [20], [42], [43], [44], [45], [46], [47], [48], [49]. Due to the high flux of the X-ray beam from the synchrotron ring, fCT allows a scan to be captured within 1 min at a pixel size of 1 μm. This allows a paste sample to be continuously scanned during the hydration process. However, the micron-sized resolutions limit does not provide detailed insights for particles <5 μm [20], [49]. Fortunately, the combination of nCT and fCT has allowed the development of fast nano X-ray computed tomography (fnCT). fnCT can capture a 3D data set in <2 min at a pixel size of 50 nm. This makes this procedure an exciting method to evaluate hydrating pastes. fnCT collects multiple X-ray radiographs at various rotation angles and generates a 3D model of the scanned sample, which is also referred to as a 3D tomography [50], [51]. In one tomography, the X-ray absorptions of different components (e.g., C 3 S and hydrates) differ as functions of density and chemistry [52], [53]. These X-ray absorption contrasts can be used to extract detailed information about the 3D microstructure [26], [54], [55]. In this paper, fnCT is used to collect time-lapse tomographs of hydrating C 3 S paste from 18 min after mixing to 7 h of hydration. The bulk measurements of anhydrous C 3 S, as well as the microstructural changes of individual C 3 S particles, are directly observed, quantified, and discussed. The dissolution behavior of C 3 S particles at various size scales is systematically analyzed and compared. This work aims to find the relationship between the size of C 3 S particle sizes and their dissolution rates. This provides significant insights into the early-age hydration of C 3 S on length and time scales not previously possible. Because of the magnitude of the data and the substantial amount of observations, this work will solely focus on the change in the anhydrous particles. Changes in the hydration products will be reported in future work.

42 ENGINEERING↗
DOE OSTI2020

UT-GOM2-2 Drilling Fluid (Technical Note)

It is proposed that a salt-saturated, water-based mud might improve borehole stability for UT-GOM2-2 relative to a fresh-water-based mud. However, the primary objective for UT-GOM2-2 is to safely and successfully acquire uncompromised hydrate-bearing sediment cores. This can only be done if conditions stay within the hydrate stability zone, and well away from the hydrate stability boundary. The addition of salt to the drilling mud, shifts the hydrate stability boundary closer to estimated conditions. This shift, by some estimates of pressure and temperature, where conditions now fall outside of the hydrate stability zone, may result in borehole enlargement and the release of free gas into the borehole. This shift by all estimates, even when coring conditions stay inside the hydrate stability zone, shrinks the window between the estimated conditions and the hydrate stability boundary. This shift is likely to compromise the hydrate-bearing cores while they are being recovered from the bottom-hole to the rig floor. In this report we present two examples: 1) Assuming temperature and pressure from in-situ estimates: Hydrate within the target reservoirs (Orange and Blue) at Walker Ridge Block 313 (WR 313) will be outside the hydrate stability zone in the presence of a drilling mud with 9.5 wt.% salinity (the salinity of the proposed 10.5 ppg salt-based mud) at in situ pressure and temperature. Thus, the hydrate will be unstable. A 10.5 ppg salt-based mud may result in dissociation of the hydrate into its components: water and gas. 10.5 ppg salt-based mud may enlarge the borehole, release free gas into the borehole, and compromise the cores. 2) Assuming temperatures equal to the measured LWD borehole temperatures at this location: Hydrate within the target reservoirs will be stable with a salinity of 9.5 wt.% (the salinity of the proposed 10.5 ppg salt-based mud), but possibly unstable (just at the methane hydrate stability boundary) for a salinity of 17.2 wt.% (the salinity of the proposed 13.5 ppg salt-based kill mud). if the borehole has the same temperature as recorded during previous LWD drilling at this location. A 13.5 ppg salt-based kill mud may destabilize the borehole. More importantly, a 10.5 ppg salt-based mud does not provide a large enough window between the estimated conditions and the hydrate stability boundary. Core temperatures and pressures fluctuate from the bottom-hole conditions as the core is brought up from the bottom-hole to the rig floor. These fluctuations are likely to cause the hydrate in the cores to touch or cross the stability boundary. Therefore, cores captured using a 10.5 ppg salt-based mud are likely to be compromised during core recovery to the rig floor.

03 NATURAL GAS↗
DOE OSTI2020

DOE Award No.: DE-FE0023919 Phase 3 Scientific/Technical Report

This is the Phase 3 Report for the ‘Deepwater Methane Hydrate Characterization and Scientific Assessment or Genesis of Methane Hydrates in the Gulf of Mexico (GOM2)’ research project (DOE Award No. DE-FE0023919). The report summarizes activities from January 16, 2018 to September 30, 2019. The project is led by the University of Texas at Austin (UT). The objective is to gain insight into the nature, formation, occurrence and physical properties of methane hydrate-bearing sediments for the purpose of methane hydrate resource appraisal through the planning and execution of drilling, coring, logging, testing and analytical activities that assess the geologic occurrence, regional context, and characteristics of marine methane hydrate deposits in the Gulf of Mexico outer continental shelf (OCS). We determined that it would not be possible to pursue the project with the International Ocean Discovery Program (IODP) and then developed a revised science and operations plan to maximize the science using a commercial vessel within the budget that is available. We improved the scientific capability of the UT pressure core center by adding the ability to X-ray pressure cores, and the ability to cut and store multiple core samples for experimental analysis. We transferred pressure cores to peer institutions, including the National Energy Technology Lab (NETL) the United States Geological Survey (USGS Woods Hole). We made advances in understanding the composition and source of gasses locked in the methane hydrate from Green Canyon 955 (GC-955). We developed approaches to determine the in-situ salinity of hydrate-bearing samples, revealing that the in situ salinity of the GC 955 reservoir is just above that of seawater. We determined that the GC-955 hydrate reservoir is composed of sandy silt with a high concentration of hydrate interbedded with clayey silt with no hydrate present. We determined that some or all of the intervals bounding the hydrate reservoir are composed of material similar to the reservoir (sandy silt with hydrate and clayey silt with no hydrate), but with a lower net to gross. We determined that the reservoir effective permeability at a hydrate saturation of ~80-90 % is ~0.1 mD (or 1.0×10-16 m2) to ~0.5 mD (or 5.0×10-16 m2) and the intrinsic permeability is ~12 mD (or 1.2×10-14 m2). The GC-955 reservoir in-situ porosity of sandy silt is 0.38 to 0.40 and is largely independent of effective stress, and that the porosity of clayey silt is 0.33 at an in situ effective stress of 3.8 MPa to ~0.37 at zero effective stress. We developed a systematic, repeatable approach to studying hydrate reservoir properties by reconstituting individual lithofacies from dissociated pressure cores. We determined index properties of GC-955 reservoir, including liquid limit and plasticity, porosity, capillary behavior, and particle size distribution. We developed a more robust pressure coring technology. We finalized and published the UT-GOM2-1 Expedition Volume and we finalized a dedicated volume on the UT-GOM2-1 expedition that will be published in the American Association of Petroleum Geologists Bulletin (AAPG) in spring 2020.

03 NATURAL GAS↗
DOE OSTI2020

Dynamic Behavior of Natural Seep Vents: Analysis of Field and Laboratory Observations and Modeling (Final Scientific/Technical Report)

In this project, we have analyzed data collected by the U.S. Department of Energy (DOE), National Energy Technology Laboratory (NETL) in a high pressure water tunnel (HPWT) and data from two research cruises to natural seeps in the Gulf of Mexico to adapt and validate a numerical model to predict the dynamics of natural seeps in the deep oceans. The HPWT data include video observations of the shrinkage rate of individual methane and natural gas bubbles under simulated deep-water conditions. Field data were collected during two cruises by the Gulf Integrated Spill Research (GISR) Consortium led by Texas A&M University and funded by the Gulf of Mexico Research Initiative (GoMRI). These data included in situ observations from a remotely operated vehicle (ROV) of gas bubbles at two natural seep sites in the Gulf and acoustic observations of the natural seep bubble flares in the ocean water column. The acoustic data were from multibeam echosounders, one mounted in a forward-looking orientation on the ROV and another mounted down-looking in the haul of the ship. All of these laboratory and field data were focused on the dynamics of natural gas bubbles at temperatures and pressures favorable for clathrate hydrate formation between the gas and water. Our analyses of this data focused on understanding the mechanisms responsible for gas bubble dissolution within the hydrate stability zone (HSZ) of the oceans. Ice-like hydrate shells may form on the bubble-water interface under these conditions, and it was unknown how this might affect the mass transfer of gas into the ocean. We were able to extract bubble shrinkage rates from the HPWT datasets. Using this data we determined that mass transfer coefficients with and without a hydrate shell match empirical values for bubbles in contaminated systems (so-called dirty bubbles contaminated by naturally occurring surfactants). We also showed that free gas, and not gas hydrate, is the dominant dissolving phase when the hydrate sub-cooling is below 11 degree Celsius (temperature difference between hydrate the hydrate formation temperature and ambient temperator) or the pressure is reducing as bubbles rise through the ocean water column. Using this mass transfer model, our numerical model of bubble dissolution matched the over 200 HPWT experiments with an average error of 10% for predicting the bubble size at the end of an experiment. From field data in the literature, we also observed that gas bubbles dissolve faster when they are initially released, following mass transfer coefficients for so-called clean-bubbles (those not yet contaminated by surfactants). Shortly after release within the HSZ, a hydrate shell forms on the bubble-water interface, and the mass transfer reduces to rates matching those of dirty bubbles. We correlated this transition time from clean to dirty bubble behavior with the initial bubble surface area and the hydrate sub-cooling. With this model for hydrate formation time and using the mass transfer coefficients deduced from the HPWT data, we validated our numerical model for predicting the rise heights of natural seep flares in the oceans. Flare heights are commonly observed in haul-mounted acoustic multibeam data. The numerical model predicts bubbles to rise high in the ocean water column owing to the slower mass transfer rates for dirty bubbles that accompany the majority of their rise time. We found that the numerical model predictions matched the observed flare heights within 5% to 10% accuracy when we compared the rise heights of the largest bubbles released from the seafloor with the bubbles acoustically visible in the multibeam data. Bubbles become acoustically transparent as they shrink to sizes of order 1 mm in diameter for the multibeam frequencies used in the field. The forward-looking multibeam on the ROV also provided data on the lateral spreading of bubbles in natural seep flares. Our analysis of this data showed that spreading follows a diffusion process, with the effective diffusivity correlating with the wobbling length scale of these ellipsoidal bubbles. When we apply this diffusivity in a random displacement model of bubble spreading, our numerical simulations match closely the lateral spread observed by the M3 in the ocean water column. Finally, we compared the seep model predictions for the acoustic properties of these natural seep plumes with that observed by the acoustic instruments in the field. The M3 and EM 302 observations were converted to relative values of target strength using a calibration we obtained in the laboratory for the M3 and using an algorithm from the manufacturer for the EM 302. Comparing the numerical seep model to these data, we obtain good agreement over the whole height of rise of these bubble flares. This further validates the numerical model. Overall, our validated seep model captures the key dynamics of gas bubbles released from natural seeps in the oceans and helps to predict the fate of methane in the water column.

03 NATURAL GAS↗
DOE OSTI2024

UT-GOM2-2 Preliminary Report: Terrebonne Basin Northern Gulf of Mexico, 30 July-28 September 2023

In the summer and fall of 2023, the Gulf of Mexico Deepwater Hydrate Coring Expedition (UT-GOM2-2) drilled, cored, made downhole measurements, and analyzed samples from the seafloor to the base of the gas hydrate stability zone in one location (Site H, WR313) in the Terrebonne basin, deepwater Gulf of Mexico. Analyses of data and samples from the expedition will inform biological, geochemical, and geomechanical models to constrain the role of gas hydrates in the carbon cycle and the potential for gas hydrates as an energy resource. Pressure and conventional cores were collected continuously to a depth of 155.1 meters below the seafloor (mbsf). At deeper depths, cores were taken periodically from hydrate-bearing sands and their bounding muds to a total depth of 861.3 mbsf. 162.6 m of conventional core and 54.8 m of pressure core were obtained. Twelve temperature measurements were made between 27.1 and 144.5 mbsf to determine the geothermal gradient. At the seafloor, more than 4 m of sandy silt of unknown origin was encountered. Beneath this sand, to a depth of ~200 mbsf, the section was composed of interbedded mud and biogenic carbonate ooze. The biogenic ooze correlated to low density and high porosity intervals observed in the previously acquired logging while drilling (LWD) data and as measured. Calcareous nannofossil biostratigraphy constrains the entire record to the Pleistocene (< 0.91 million years) with a pronounced increase in sedimentation rate with depth. Beneath 200 mbsf, the section was predominantly composed of mud with two thicker, hydrate-bearing coarse-grained intervals, which are commonly known as the Blue and Orange sands. The dissolved gas concentration was quantified from pressure cores. In the shallow section, dissolved methane concentration increased below the sulfate-methane transition zone (SMTZ) and reaches saturation (the limit of solubility for methane) at 147 mbsf. Gas expansion was very common in conventional and depressurized pressure (conventionalized) cores below the SMTZ. At deeper depths, the methane concentration within muds bounding the Blue and Orange reservoirs was generally found to be less than saturation. The dissolved and hydrate gas composition is consistent with a microbial source, containing greater than 99.99% methane and only trace concentrations of ethane, propane, and butane. The methane to ethane ratio (C 1 /C 2 ) and the methane to ethane plus propane (C 1 /(C 2 +C 3 )) decrease with depth down to at least 678 mbsf, mainly driven by the increase in ethane with depth. It is unclear if this trend continues through the Orange sand interval. The δ 13 C isotopic signature of methane ranges between -69.9 and -78.5 ‰ Vienna Pee Dee Belemnite (VPDB). Pressure core recovery of all sandy intervals was poor. However, pressure core logs of the Orange sand show intervals of low density and high velocity, which are indicative of high hydrate saturation. One core from within the Orange sand was composed of interbedded graded sandy silt and mud. The sandy silts from this core are composed of mainly quartz and feldspar with some lithics. Most of the recovered pressure core samples are maintained at near in-situ pressure and temperature (within the hydrate stability field) at the University of Texas Pressure Core Center awaiting analysis. In the shallow section, samples will be used to determine the flux of organic carbon through the basin system, find the rate at which that carbon was consumed, and understand the microbial population responsible for these processes. In the deeper section, samples from in and around the hydrate reservoirs will be used to determine the petrophysical properties of the reservoir and bounding seals in these systems.

03 NATURAL GAS↗
DOE OSTI2021

DOE Award No.: DE-FE0023919 Phase 4 Scientific/Technical Report

This is the Phase 4 Report for the ‘Deepwater Methane Hydrate Characterization and Scientific Assessment or Genesis of Methane Hydrates in the Gulf of Mexico (GOM2)’ research project (DOE Award No. DE-FE0023919). The report summarizes activities from October 1, 2019 to September 30, 2020. The project is led by the University of Texas at Austin (UT). The project objective is to gain insight into the nature, formation, occurrence and physical properties of methane hydrate-bearing sediments for the purpose of methane hydrate resource appraisal through the planning and execution of drilling, coring, logging, testing and analytical activities that assess the geologic occurrence, regional context, and characteristics of marine methane hydrate deposits in the Gulf of Mexico outer continental shelf (OCS). We published a dedicated American Association of Petroleum Geologists Bulletin volume describing initial results from the UT-GOM2-1 expedition in Sept. 2020. This is part 1 of a multi-volume commitment by AAPG to this project. We further confirmed that the natural gas in hydrate at GC-955 was formed by primary microbial processes (>76.1 %). The in-situ effective permeability hydrate-bearing sandy silts at the GC-955 reservoir ranges from 0.1 md (1.0×10-16 m2) to 2.4 md (2.4×10-15m2) in cores with 83% to 93% hydrate saturation. The intrinsic permeability (the single phase permeability) is estimated from reconstituted samples to be ~12 md (1.2×10-14 m2) to ~41 md (4.1×10-14 m2). We used observation and models to interpret that the core degradation that is found in pressure cores is due to dissociation of the methane hydrate in the outer circumference of the core and dissolution of that methane into the fresh pore water that the core is stored with. We are designing approaches to minimize this core loss in the future. We spent an enormous amount of effort to further improve the ability of the pressure coring tool (the PCTB) to pressure seal correctly. We completed upgrading the upper section of the PCTB to address poor pressure. We successful tested the modifications at Geotek’s test facility in Salt Lake City (Bench Test II). We completed a Land Test of the PCTB at the Schlumberger Cameron Test and Training Facility (CTTF). The tool did not seal in 6 out of 7 tests and we clearly demonstrated that cuttings were wedging in the ball valve assembly, keeping the ball valve from sealing. We reproduced the failure mechanism observed during the land test at Salt Lake City and confirmed the sensitivity of the ball valve assembly to grit. Geotek designed and tested 9 modifications to address this issue and the PCTB is now 100% successfully sealing in the presence of grit. Our science expedition is scheduled for spring 2022 and we are fully focused on preparing for this. UT and Ohio State completed a Shallow Hazard Assessment report for each proposed UT-GOM2-2 drilling location, pursuant to 30 CFR 250.214(f) and 250.244 (f). The Shallow Hazard Reports will accompany the UT-GOM2-2 Exploration Plan that is submitted to BOEM, and completes the geological and geophysical analysis for UT-GOM2-2 permitting efforts. We updated the UT-GOM2-2 Operations Plan (Version 1). We completed the UT-GOM2-2 Science and Sample Distribution Plan (Version 1). We evaluated the scope, budget, and schedule that would result from using a commercial vessel. We developed detailed drilling schedule, mud volume, and resource estimates. We developed a vessel specification document and a well plan, and sent these documents to prospective vessel contractors.

03 NATURAL GAS↗