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At least 1,171 records · Page 65
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Application of Electron Backscatter Diffraction to evaluate the ASR risk of concrete aggregates

Alkali-Silica Reaction (ASR) is a frequent cause of reduced concrete durability. Eliminating the application of alkali reactive aggregates would reduce the quantity of ASR concrete deterioration in the field. This study introduces an Electron Backscatter Diffraction (EBSD) technique to distinguish the ASR risk of slow-late reacting aggregates by measuring microstructural properties of quartz. Quantifying the amount of quartz grain boundaries and the associated misorientation of grains can thereby be used to differentiate microstructures bearing an ASR risk. It is also shown that dissolution of quartz in high pH environments occurs along quartz grain and subgrain boundaries. Results of EBSD analysis are compared with ASR performance testing on concrete prisms and optical light microscopy characterization of quartz microstructure. EBSD opens new possibilities to quantitatively characterize microstructure of quartz in concrete aggregates with respect to ASR. This leads to a better understanding on the actual cause of ASR.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Transformations of Na, Al, Si and Fe species in red mud during synthesis of one-part geopolymers

Reaction mechanism of one-part geopolymer formation using red mud (RM) was explored in this study. Leaching test, X-ray photoelectron spectroscopy (XPS), Mössbauer spectroscopy and nitrogen isothermal adsorption (NIA) were conducted to study transformations of Na, Al, Si, Fe species, binding energies of Al−O and Si−O, and pore structure, respectively. The alkali-thermal-activated RM could dissolve in water to release large amounts of soluble Na, Al and Si species for geopolymerization. But more dissolved Si is needed from added silica fume (SF) to form stable geopolymer gels. The binding energies of Al−O and Si−O bonds in the geopolymer increased with the polymerization of reactive SiO{sub 2} and Al{sub 2}O{sub 3}. The coordinated Fe{sup 3+} in RM played a role like Al{sup 3+} by replacing it in the aluminosilicates structure, and exerted no obvious impact on geopolymerization. The dissolved SF took part in the geopolymerization to form dense geopolymer matrices in long-term curing. - Highlights: • Large amounts of Na, Al and Si dissolved from alkali-thermal-activated RM in water. • Low Si/Al geopolymers will dissolve and release soluble Al in long-term curing. • Dissolved Si from SF participates in the polymerization of soluble Na, Al and Si. • The binding energies of Al−O and Si−O will increase after geopolymerization. • The coordinated Fe{sup 3+} replaces Al{sup 3+} in aluminosilicate structure of geopolymer.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Isothermal calorimetry and in-situ XRD study of the NaOH activated fly ash, metakaolin and slag

Much is unknown about the reaction processes responsible for the formation and polycondensation of geopolymers and other alkali activated materials. In this work, isothermal calorimeter and in-situ XRD were adopted to study the heat and mineral evolution of NaOH activated fly ash, metakaolin and ground granulated blast furnace slag. Both activator concentration and temperature have profound influences on duration of exothermal geopolymerization peaks. NaOH activated fly ash is more temperature dependable, with much higher activation energy than metakaolin and slag. The dissolution of source precursor is rapid and the formation of new phases can be detected by the end of the initial dissolution period. The in-situ XRD measurement together with the PONKCS analysis method promotes quantitative estimation of amorphous evolution during alkali activation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Pozzolanic reactivity of natural pozzolans, ground glasses and coal bottom ashes and implication of their incorporation on the chloride permeability of concrete

It is well understood that the partial replacement of portland cement with pozzolans in sufficient proportions results in improved long-term performance of concrete. However, dwindling availability of the most widely used pozzolan in the construction industry, fly ash, is forecast due to the termination of coal-fired electricity power stations around the world, necessitating the exploration of alternative pozzolans. Experimental investigations are conducted to study the performance of traditional pozzolans such as fly ash, silica fume and natural pozzolans (metakaolin, pumice, perlite and lassenite) together with novel pozzolans, including ground glasses (high-alkali and low-alkali), and ground bottom ash. Twenty-one concrete mixtures are examined for compressive strength, electrical conductivity, electrical resistivity, chloride permeability, and chloride migration coefficient. The reactivity of pozzolans studied is also determined in terms of compressive strength in lime-pozzolan mortar using a modified lime-reactivity test method. Many of the materials tested demonstrate the potential to be used in place of fly ash. However, a wide variation in the performance of these materials is evident which highlights the need for a reliable test to determine the level of reactivity of a pozzolan. The results indicate that the 7-day strength in the modified lime-reactivity test provides a good indication of the pozzolanic reactivity of the material and of how the material can be expected to contribute to the strength and permeability of concrete. The use of electrical resistivity as an indicator of the performance of pozzolans in terms of strength development and chloride penetration resistance when used to partially replace portland cement in concrete is also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Sorption and electrokinetic properties of ASR product and C-S-H: A comparative modelling study

Alkali-silica reaction (ASR) is one of the most important concrete durability issues worldwide. ASR products formed at high temperature have a structure similar to the natural mineral shlykovite. Reactive Grand Canonical Simulations were used to investigate sorption of K{sup +}, Cl{sup −} and Ca{sup 2+} on C-S-H and ASR products at different pH (10.0 to 13.0) and pore water chemistry. Divalent ions can overcompensate for the negative surface charge, in particular for C-S-H, which leads to a co-adsorption of negative species such as Cl{sup −}. At high K/Ca in solution, monovalent K{sup +} can desorb calcium from C-S-H and shlykovite surface. The calculated Ca/K partition coefficient shows a higher affinity of ASR product for K{sup +}, while C-S-H favours Ca{sup 2+}. The uptake of K{sup +} by ASR products lowers the alkali concentration in the solution and could thus slow down the rate of ASR.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Formulation of low clinker blended cements and concrete with enhanced fresh and hardened properties

Blended cements appear as the most promising way to massively produce cements with reduced environmental footprints. However, considering the generally lower early mechanical performance of highly blended cements, chemical admixtures are increasingly relied upon to increase early strength. However, in many cases this can negatively impact other properties as rheology and durability. This paper proposes an approach to formulate low clinker cements and concrete using moderate alkali activation or gypsum to enhance early and long-term compressive strength, without inducing excessive alkali-silica reaction (ASR) expansion. It examines blended cements containing burnt oil shale along with limestone and fly ash or slag as supplementary cementitious materials. It optimizes the combination of polycarboxylate ether (PCE) superplasticizers with the strength enhancers. Along with the use of Ca(NO{sub 3}){sub 2} to drive PCE adsorption, this provides good rheology control, increased early and long-term compressive strength, as well as acceptable ASR expansion in cements with only 50% clinker.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Determination of transition metal ions in fossil fuel associated wastewaters using chelation ion chromatography

Here, this study outlines the development and subsequent validation of a method using chelation ion chromatography (CIC) pretreatment followed by traditional ion chromatography (IC) and post column UV/vis detection to measure transition metals in fossil fuel wastewaters, such as oil & gas (O&G) brines and coal mine drainage (CMD) waters. Measurement of transition metals is often an important characterization step in the research of environmental and energy systems. IC represents one way to measure these metals with the advantages of being versatile, simple and relatively low cost compared to other analytical methods. However, high concentrations of alkali and alkaline earth metals present in fossil fuel wastewaters will decrease IC detectability of transition metals in these waters. In this study, a CIC method was developed for the analysis of transition metal ions (Fe 3+ , Cu 2+ , Ni 2+ , Zn 2+ , Co 2+ , Mn 2+ , and Fe 2+ ) in fossil fuel associated wastewaters such as Appalachian CMD and O&G wastewaters from the Permian and Bakken shale basins in the United States. CIC system incorporated an on-line chelator column (e.g., the MetPac CC-1) with high selectivity for transition metals over alkali and alkaline earth metals for salt matrix removal prior to transition metal separation and detection. Additional method developments also included acidifying all samples to 2% v/v HCl and using gradient elution rather than isocratic. The recoverability of transition metals in simple salt solutions commonly found in CMD and brine samples (e.g. NaCl, Na 2 SO 4 , CaCl 2 ) using CIC was evaluated and compared to that using traditional IC. Our results found that the CIC system significantly improved transition metal recoveries for samples in 10,000 mg/L CaCl 2 matrix, reaching 87%-108% recovery for all analytes, as opposed to 2-323% recovery in traditional IC. The limits of detection in this study achieved 10.09 – 161.2 μg/L, comparable to reported values in similar IC studies. The developed method was also verified with certified water samples, resulting in 89% - 111% recoveries in samples with higher analyte concentrations (i.e. >4x the LoDs). The developed method achieved 87% -112% recoveries for most analytes in CMD samples and 72%-138% recoveries for Bakken shale samples, relative to ICP-MS values. Overall, the current IC method can be a very good screening tool for fast and cheap analysis for transition metals at mg/L level, to facilitate selection of samples for more detailed ICP-MS analysis.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2024

Chemo-Mechanical Instabilities in Lithium Cobalt Oxide at Higher State-Of-Charge in Li-Ion Batteries

Transition metal oxide cathodes are widely used in commercial Li-ion batteries. However, their practical charge capacity is limited due to severe chemo-mechanical instabilities at higher charge voltage, and state-of-charge condition. Here, in situ stress and strain measurements were synchronized to probe mechanical deformations in the lithium cobalt oxide (LCO) cathode via a multi-beam stress sensor and digital image correlation, respectively. In situ mechanical measurements revealed how Li removal from the electrode structure induces deformations on the LCO composite cathodes during cycling. The structure and morphology of the LCO cathodes were further investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies. Two distinct electrochemical and mechanical behaviors were identified when the LCO was charged up to 4.65 V. The LCO undergoes a compressive stress generation when charged up to 4.2 V and surface fractures on the LCO particles were detected by SEM. LCO cathode experienced significantly large contractions (negative strains) when charged up to 4.65 V, where intergranular crack formation and phase transformation were detected on the LCO particles via SEM and XRD, respectively. Overall, the study bridges complicated structural deformations with in situ analysis of mechanical degradations in LCO cathodes charged at higher voltages. The correlation is vital to understanding instability mechanisms in transition metal oxides at high voltages for alkali metal ion batteries.

higher state-of-charge↗
DOE OSTI2025

Impact of low-chemical storage pretreatment of loblolly pine bark on biochar from microwave pyrolysis

Forest product residues such as bark represent a low-cost, abundant feedstock for bioenergy, but their high ash and alkali and alkaline earth metal (AAEM) content limit thermochemical conversion efficiency. This study evaluates the use of low-severity chemical pretreatments during anaerobic storage to improve the performance of microwave pyrolysis for loblolly pine bark. Bark was treated with dilute sulfuric acid (0.1% and 1%, w/w) or sodium hydroxide (4%, w/w) and incubated anaerobically for one or two weeks to simulate in-pile biorefinery storage. The most effective treatment—1% H2SO4 for two weeks—reduced AAEM content by 35.7% and increased bio-oil yield by 11% compared to untreated controls, while also reducing pyrolysis gas production. In contrast, alkali treatment did not reduce AAEM levels and led to decreased bio-oil yields with increased gas formation. Although biochar yields were relatively stable across treatments, their physicochemical characteristics varied significantly. Acid-treated bark yielded biochars with higher carbon content, lower O/C and H/C ratios, greater surface area, and enhanced heating values. These improvements suggest that chemical pretreatment during storage can tailor biochar quality for specific end uses. Biochars produced under optimized conditions exhibited properties suitable for soil amendment, carbon sequestration, and solid fuel applications. This integrated approach—combining storage, mild chemical conditioning, and microwave pyrolysis—provides a viable pathway to enhance the value and sustainability of bark-derived bioenergy products.

09 - BIOMASS FUELS↗
DOE OSTI2016

Performance assessment of dilute-acid leaching to improve corn stover quality for thermochemical conversion

Lignocellulosic biomass is a sustainable energy source that can help meet the increasing demand for biofuels in the United States. However, the quality and availability of such feedstocks greatly affects their suitability for downstream conversion. This work reports the effects of dilute-acid leaching at various solid loadings, temperatures and acid loadings on the quality of a traditional biochemical feedstock, corn stover, as a potential feedstock for thermochemical conversions. At 5 wt% solids, dilute-acid leaching was observed to effectively remove 97.3% of the alkali metals and alkaline earth metals that can negatively affect degradation pathways during pyrolysis and result in greater yield of non-condensable gases. In addition, up to 98.4% of the chlorine and 88.8% of the phosphorus, which can cause equipment corrosion and foul upgrading catalysts, respectively, were removed. At 25°C in the absence of acid, only 6.8% of the alkali metals and alkaline earth metals were removed; however 88.0% of chloride was still removed. The ratio of alkaline/acidic ash species has been suggested to proportionately relate to slagging in biopower applications. The initial alkali/acid ratio of the ash species present in the untreated corn stover was 0.38 (significant slagging risk). At 5 wt% solids, this ratio was decreased to 0.18 (moderate slagging risk) at 0 wt% acid and 90°C, and was decreased to 0.07, 0.08 and 0.06 at 0.5 wt% acid at 25°C, 50°C and 90°C, respectively (little or no slagging risk). Increasing the acid loading to 1.0% only slightly decreased the measured alkali/acid ratio of remaining ash species. Lastly, the results presented here show that a water wash or dilute-acid preprocessing step can improve corn stover quality for pyrolysis, hydrothermal liquefaction and biopower.

09 BIOMASS FUELS↗
DOE OSTI2025

Hydrogen-rich syngas production from the steam co-gasification of low-density polyethylene and coal refuse

Gasification provides a promising pathway for transforming waste materials into valuable products, such as fuels and chemicals. Here, this study investigates the steam co-gasification of low-density polyethylene (LDPE) and compressed thickener underflow, representative of coal refuse (CR), in a drop tube reactor. The effects of feed blend ratio (0–100 wt% LDPE) and temperature (800–1000 °C) on syngas composition, tar formation, and process efficiency are examined. The high volatility of LDPE makes it more reactive than CR but also promotes the formation of 2–7 ring aromatic tars. Increasing temperature improves carbon conversion efficiency (CCE), cold gas efficiency (CGE), and syngas yield, although the lower heating value (LHV) of syngas decreases. Hydrogen is the dominant gas product, reaching 59 vol% with the H 2 /CO molar ratio ranging from 2.27 to 4.74. Synergistic effects from alkali and alkali earth metals (AAEMs), particularly K and Ca, in CR ash enhance syngas yield by catalyzing char gasification and tar cracking. Hematite (Fe 2 O 3 ) and ash from sub-bituminous/bituminous coals are explored as tar reforming catalysts. Fe 2 O 3 achieves 100 % tar reforming efficiency, while coal ash, with a lower Fe 2 O 3 content (15 wt%), is less effective at cracking polycyclic aromatic hydrocarbons, particularly naphthalene. These findings demonstrate the flexibility of co-gasification, allowing precise tuning of syngas characteristics for specific downstream applications. Further optimization of waste-derived catalysts could enhance the economic viability of gasification in waste-to-energy processes.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

On the dissolution of a borosilicate glass with the use of isotopic tracing – Insights into the mechanism for the long-term dissolution rate

An understanding of the mechanisms responsible for controlling the long-term corrosion rate of nuclear waste glass is paramount if reliable glass dissolution models are to be used to calculate the controlled release of radionuclides from nuclear waste glass under geologic disposal conditions. Additionally, understanding silicate glass dissolution is also important for natural glasses to understand the role from the dissolution of these glasses has on the composition of natural aquatic systems. Two general mechanisms appear to be responsible for the elemental release from glass to the surrounding biosphere - ion exchange (release principally of alkalis) and matrix dissolution (release of the structural components of the glass). Key unknowns related to these mechanisms are the impact of surface layers on the altered glass and how these layers participate in corrosion. To better understand the impact of these layers on glass corrosion, we made two glasses of the same elemental composition, but with selected elements enriched in specific isotopes, e.g. more 10 B than 11 B. We reacted these glasses for 1 y then the solutions from each were exchanged and the chemistry of the solutions and the solids were followed for another 2 y and in some cases 3 y. This allowed us to follow changes in the glasses with respect to these elements and how these elements were transported through the alteration layers with time and, for at least one element, into the glass. Results from these experiments demonstrate that the release behavior of different elements is strongly dependent on their structural role in the glass (e.g. network formers and modifiers), but, more importantly, the role of water transport and subsequent ion exchange has in the long-term dissolution of the glass studied here. In this article, we highlight the behavior of four elements: lithium, sodium, silicon, and boron. Lithium and sodium, network modifying elements, have similar chemistries. The behavior of Li could be tracked in more detail by following both 6 Li and 7 Li; Li penetrates through the gel layer in both directions without hinderance and into and released from the glass deeper than sodium. Silicon, a network forming element, reacts with the silica-rich alteration layer. Boron, a network forming element, does not accumulate in the gel or the pristine glass and has a very sharp elemental profile between the pristine glass and alteration layer. Boron, lithium, and sodium elemental profiles suggest that there is little if any transport control within the alteration layer. The correlation between the Li and Na profiles and that of a water species suggest that the limiting release is a steady state between the diffusion of a water species and matrix dissolution that results in a low release rate for alkali and this provides a steady driving force for the long-term dissolution of glass.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Classification scheme for sedimentary and igneous rocks in Gale crater, Mars

Rocks analyzed by the Curiosity rover in Gale crater include a variety of clastic sedimentary rocks and igneous float rocks transported by fluvial and impact processes. Here, to facilitate the discussion of the range of lithologies, we present in this article a petrological classification framework adapting terrestrial classification schemes to Mars compositions (such as Fe abundances typically higher than for comparable lithologies on Earth), to specific Curiosity observations (such as common alkali-rich rocks), and to the capabilities of the rover instruments. Mineralogy was acquired only locally for a few drilled rocks, and so it does not suffice as a systematic classification tool, in contrast to classical terrestrial rock classification. The core of this classification involves (1) the characterization of rock texture as sedimentary, igneous or undefined according to grain/crystal sizes and shapes using imaging from the ChemCam Remote Micro-Imager (RMI), Mars Hand Lens Imager (MAHLI) and Mastcam instruments, and (2) the assignment of geochemical modifiers based on the abundances of Fe, Si, alkali, and S determined by the Alpha Particle X-ray Spectrometer (APXS) and ChemCam instruments. The aims are to help understand Gale crater geology by highlighting the various categories of rocks analyzed by the rover. Several implications are proposed from the cross-comparisons of rocks of various texture and composition, for instance between in place outcrops and float rocks. All outcrops analyzed by the rover are sedimentary; no igneous outcrops have been observed. However, some igneous rocks are clasts in conglomerates, suggesting that part of them are derived from the crater rim. The compositions of in-place sedimentary rocks contrast significantly with the compositions of igneous float rocks. While some of the differences between sedimentary rocks and igneous floats may be related to physical sorting and diagenesis of the sediments, some of the sedimentary rocks (e.g., potassic rocks) cannot be paired with any igneous rocks analyzed so far. Finally, in contrast, many float rocks, which cannot be classified from their poorly defined texture, plot on chemistry diagrams close to float rocks defined as igneous from their textures, potentially constraining their nature.

58 GEOSCIENCES↗
DOE OSTI2017

Classification of igneous rocks analyzed by ChemCam at Gale crater, Mars

Several recent studies have revealed that Mars is not a simple basalt-covered planet, but has a more complex geological history. In Gale crater on Mars, the Curiosity rover discovered 59 igneous rocks. This article focuses on their textures (acquired from the cameras such as MAHLI and MastCam) and their geochemical compositions that have been obtained using the ChemCam instrument. Light-toned crystals have been observed in most of the rocks. They correspond to feldspars ranging from andesines/oligoclases to anorthoclases and sanidines in the leucocratic vesiculated rocks. Darker crystals observed in all igneous rocks (except the leucocratic vesiculated ones) were analyzed by LIBS and mainly identified as Fe-rich pigeonites and Fe-augites. Iron oxides have been observed in all groups whereas F-bearing minerals have been detected only in few of them. From their textural analysis and their whole-rock compositions, all these 59 igneous rocks have been classified in five different groups; from primitive rocks i.e. dark aphanitic basalts/basanites, trachybasalts, tephrites and fine/coarse-grained gabbros/norites to more evolved materials i.e. porphyritic trachyandesites, leucocratic trachytes and quartz-diorites. The basalts and gabbros are found all along the traverse of the rover, whereas the felsic rocks are located before the Kimberley formation, i.e. close to the Peace Vallis alluvial fan deposits. This suggests that these alkali rocks have been transported by fluvial activity and could come from the Northern rim of the crater, and may correspond to deeper strata buried under basaltic regolith (Sautter et al., 2015). Some of the basaltic igneous rocks are surprisingly enriched in iron, presenting low Mg# similar to the nakhlite parental melt that cannot be produced by direct melting of the Dreibus and Wanke (1986) martian primitive mantle. The basaltic rocks at Gale are thus different from Gusev basalts. They could originate from different mantle reservoirs, or they could have undergone a more extensive fractional crystallization. Lastly, Gale basaltic rocks could have been the parental magma of residual liquid extending into alkali field towards trachyte composition as magma fractionated under anhydrous condition on its way to the surface before sub adiabatic ascent.

58 GEOSCIENCES↗
DOE OSTI2018

Influence of hydrophilic groups and metal-ion adsorption on polymer-chain conformation of amidoxime-based uranium adsorbents

In this study, we focus on the influence of hydrophilic groups and metal-ion loading on adsorbent polymer conformation, which controls access to adsorption sites and may limit adsorption capacity. Gaining a better understanding of the factors that influence conformation may yield higher-capacity adsorbents. Polyamidoxime (PAO), deuterated-PAO polyacrylic acid diblock copolymers (d-PAO-b-PAA), and randomly configured copolymers (PAO-co-PAA) were synthesized and characterized by neutron reflectometry in air and D 2 O. For d-PAO-b-PAA, characterization was also performed after alkali conditioning and in simulated seawater. PAO and PAO-co-PAA, with similar molecular weight and grafting density, extended from 95-Å thickness in air to 180 and 280-Å in D 2 O, respectively. This result suggests that polymer swelling may cause the additional adsorption capacity observed when polymer hydrophilicity increases. Two d-PAO-b-PAA samples, A and B, with a d-PAO thickness of 55-Å swelled to 110-Å and 140-Å, respectively, with an overall thickness increase of ~160% in D 2 O. After alkali conditioning, molecular interactions increased the density of PAA near the PAO-PAA interface, while the d-PAO thickness only decreased by ~10 Å. The d-PAO thickness of both samples declined to ~90-Å after adsorption in simulated seawater due to polymer-chain crosslinking. In conclusion, these results are expected to aid in improving adsorbent synthesis to increase uranium capacity.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2015

Preparation and characterization of a hybrid alkaline binder based on a fly ash with no commercial value

Alkali-activated Portland fly ash cement (FA/OPC) and alkali activated blast furnace slag-fly ash cement (FA/GBFS) were prepared using 70% of a low quality fly ash (FA). The low quality is associated with a high content of unburned material (loss of ignition of 14.6%). The hybrid cements were activated by the alkaline solution in order to obtain an overall SiO 2 /Al 2 O 3 molar ratio of 5.0 and 6.0 and unique overall Na 2 O/SiO 2 molar ratio of 0.21. The microstructural characterization of the blended pastes generated in the systems showed the coexistence of amorphous gels C-A-S-H and N-A-S-H gels in the hybrid systems. The addition of OPC or GBFS increases the compressive strength (at 28 days of curing) up to 127% compared with the geopolymer systems based only on FA used in this study. The content of silicates soluble also plays an important role in the reaction products and higher SiO 2 /Al 2 O 3 lead to obtain higher mechanical performance and denser structure. The results obtained show that these hybrid cements are an effective way for valorization the waste used in this study for the production of high strength and low-carbon footprint cement-type material.

36 MATERIALS SCIENCE↗