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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 109 records · Page 6

The Role of Cooperative Interactions Among Surfaces, Solvents, and Reactive Intermediates on Catalysis at Liquid–Solid Interfaces (Final Report DE-SC0020224)

This project established quantitative links between inner‑sphere chemistry (active metal identity, coordination, and zeolite topology) and outer‑sphere organization (solvent identity, hydrogen‑bond networks, and pore condensation) that govern rates, activation barriers, and selectivities for alkene epoxidation and epoxide ring‑opening at solid–liquid and quasi‑liquid–solid interfaces. We deconvoluted contributions from covalent interactions at active sites and noncovalent, solvent‑mediated interactions within pores by pairing well‑defined metal substituted zeolites with controlled solvent environments. We then mapped those contributions onto measurable kinetics (ΔH‡, ΔS‡), adsorption thermodynamics (ITC), and in situ spectroscopy. The transferrable outcomes include a set of design rules that include the following understandings. First, tune silanol ((SiOH)x) density and pore topology to organize solvent networks that selectively stabilize transition states. Second, exploit activity‑coefficient‑normalized rates and adsorption– barrier correlations to diagnose when solvent reorganization rather than surface chemistry limits performance. Third, use partial pore condensation (e.g., acetonitrile, water but also generalizable to other solvents) to elicit liquid‑like stabilization effects even in nominally vapor‑phase reactors. Collectively, these results provide strategies to increase epoxidation rates, improve oxidant utilization (i.e., selectivities), and steer regioselectivity in zeolite‑based catalytic processes relevant to sustainable oxidation chemistry. These outcomes should be transferable to other classes of reactions that proceed in microporous materials and under confinement provided by organized solvents (e.g., electrochemical double layers).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Peeling back the layers: Investigating the effects of polyelectrolyte layering on surface structure and stability of oil-in-water nanoemulsions

Layer-by-layer deposition of polyelectrolytes is a useful technique for modifying surface functionalities. For drug delivery systems, alternating layers of biopolymers coat nanoemulsions, which house and protect the cargo until the time and destination of delivery. In this report we investigate molecular factors contributing to the stability and interfacial properties of nanoemulsions prepared by a co-adsorption of polymers poly(styrene sulfonate) and polyethylenimine (PEI), and surfactant dodecyltrimethylammonium bromide. We hypothesize the interplay between electrosteric and hydrophobic effects upon multi-polymer co-adsorption contributes to both macroscopic and molecular-level interfacial properties of nanoemulsions. To probe interfacial layering properties, we use vibrational sum frequency scattering spectroscopy with ζ -potential measurements to determine the adsorptive behavior and molecular conformational arrangement of the polymer layers. Complementing these interfacial studies are dynamic light scattering experiments measuring the nanoemulsion size distribution and polydispersity index over a 30-day period. Our light scattering, ζ -potential, and spectroscopic results of the nanoemulsion surface show that the duration of droplet stability and the degree of molecular orientation of adsorbed polymers can be tuned by surfactant concentration, PEI concentration, and pH. These results illustrate how molecular surface properties of multi-polymer coated nanoemulsions contribute to synergistic effects and droplet stability, enabling advancements in applications surrounding biopharmaceuticals, cosmetics, and food sciences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Atomically Dispersed Copper Sites in a Metal–Organic Framework for Reduction of Nitrogen Dioxide

Metal-organic framework (MOF) materials provide an excellent platform to fabricate single-atom catalysts due to their structural diversity, intrinsic porosity, and designable functionality. However, the unambiguous identification of atomically dispersed metal sites and the elucidation of their role in catalysis are challenging due to limited methods of characterization and lack of direct structural information. Here, we report a comprehensive investigation of the structure and the role of atomically dispersed copper sites in UiO-66 for the catalytic reduction of NO 2 at ambient temperature. The atomic dispersion of copper sites on UiO-66 is confirmed by high-angle annular dark-field scanning transmission electron microscopy, electron paramagnetic resonance spectroscopy, and inelastic neutron scattering, and their location is identified by neutron powder diffraction and solid-state nuclear magnetic resonance spectroscopy. The Cu/UiO-66 catalyst exhibits superior catalytic performance for the reduction of NO 2 at 25 °C without the use of reductants. A selectivity of 88% for the formation of N2 at a 97% conversion of NO 2 with a lifetime of >50 h and an unprecedented turnover frequency of 6.1 h-1 is achieved under nonthermal plasma activation. In situ and operando infrared, solid-state NMR, and EPR spectroscopy reveal the critical role of copper sites in the adsorption and activation of NO 2 molecules, with the formation of {Cu(I)···NO} and {Cu···NO 2 } adducts promoting the conversion of NO 2 to N 2 . This study will inspire the further design and study of new efficient single-atom catalysts for NO 2 abatement via detailed unravelling of their role in catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Interplay between Facets and Defects during the Dissociative and Molecular Adsorption of Water on Metal Oxide Surfaces

Both surface terminations and defects play a central role in determining how water interacts with metal oxides, thereby setting important properties of the interface that govern reactivity such as the type and distribution of hydroxyl groups. However, the interconnections between facets and defects remain poorly understood, limiting the usefulness of conventional notions such as that hydroxylation is controlled by metal cation exposure at the surface. Here, using hematite (α-Fe 2 O 3 ) as a model system, we show how oxygen vacancies overwhelm surface cation-dependent hydroxylation behavior. Synchrotron-based ambient-pressure X-ray photoelectron spectroscopy was used to monitor the adsorption of molecular water and its dissociation to form hydroxyl groups in situ on (001), (012), or (104) facet-engineered hematite nanoparticles. Supported by density functional theory calculations of the respective surface energies and oxygen vacancy formation energies, the findings show how oxygen vacancies are more prone to form on higher energy facets and induce surface hydroxylation at extremely low relative humidity values of 5 x10 - 5 %. Further, when these vacancies are eliminated, the extent of surface hydroxylation across the facets is as expected from the areal density of exposed iron cations at the surface. These findings help answer fundamental questions about the nature of reducible metal oxide-water interfaces in natural and technological settings and lay the groundwork for rational design of improved oxide-based catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding solvent effects on adsorption and protonation in porous catalysts

Abstract Solvent selection is a pressing challenge in developing efficient and selective liquid phase catalytic processes, as predictive understanding of the solvent effect remains lacking. In this work, an attenuated total reflection infrared spectroscopy technique is developed to quantitatively measure adsorption isotherms on porous materials in solvent and decouple the thermodynamic contributions of van der Waals interactions within zeolite pore walls from those of pore-phase proton transfer. While both the pore diameter and the solvent identity dramatically impact the confinement (adsorption) step, the solvent identity plays a dominant role in proton-transfer. Combined computational and experimental investigations show increasingly favorable pore-phase proton transfer to pyridine in the order: water < acetonitrile < 1,4 – dioxane. Equilibrium methods unaffected by mass transfer limitations are outlined for quantitatively estimating fundamental thermodynamic values using statistical thermodynamics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Transient Studies of CO 2 Adsorption over CeO 2 Nanostructures with In Situ DRIFTS and Modulation Excitation

Experiments of in-situ DRIFTS combined with modulation excitation (ME) spectroscopy showed a rich surface chemistry associated with the adsorption of CO 2 on nanocubes and nanospheres of ceria. The nanocubes exposed faces with a (100) orientation, with the edges and corners displaying (110) and (111) orientations, respectively. Here, the nanospheres mainly contained ceria (111) and (110) planes. DFT calculations showed that CO 2 is a multidentate adsorbate on ceria that can undergo changes in its bonding configuration depending on the chemical environment. At 250 °C, a temperature typically used for the conversion of CO 2 into oxygenates, alkanes and olefins, CO 2 reacted with O centers or OH groups present on the nanocubes and nanospheres to yield bi- and tri-dentate carbonates, hydroxycarbonates, and formates. Both nanostructures were highly reactive and a dynamic equilibrium was established: carbonate species were rapidly generated upon the injection of CO 2 and they decomposed upon the removal of CO 2 from the gas phase. In the case of the ceria nanocubes, the adsorption/desorption processes were essentially reversible, opening the door to catalytic transformations. A larger concentration of defects in the ceria nanospheres led to strongly bound carbonates and formates that may be spectators, site blockers, or surface modifiers in catalytic processes. In the ME studies, additional intermediates were detected, and it was clear that the response of surface species to the presence/absence of CO 2 was highly dependent on the morphology of the ceria nanostructures.

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Capture of Iodine from Nuclear-Fuel-Reprocessing Off-Gas: Influence of Aging on a Reduced Silver Mordenite Adsorbent after Exposure to NO/NO 2

Iodine radioisotopes released during nuclear fuel reprocessing must be removed from the off-gas stream before discharge. One promising material for iodine capture is reduced silver mordenite (Ag 0 Z). Nevertheless, the adsorbent’s capacity will degrade, or age, over time when the material is exposed to other off-gas constituents. Though the overall impact of aging is known, the underlying physical and chemical processes are not. To examine these processes, Ag 0 Z samples were prepared and aged in 2% NO 2 in dry air and in 1% NO in N 2 gas streams at 150 °C for up to six months. Aged samples were then characterized using scanning electron microscopy, X-ray diffraction, Raman spectroscopy, and X-ray absorption spectroscopy. These techniques show that aging involves two overarching processes: (i) oxidation of the silver nanoparticles present in Ag 0 Z and (ii) migration of oxidized silver into the mordenite’s inner network. Silver on the nanoparticle’s surface is oxidized through adsorption of O 2 , NO, and NO 2 . Additionally, Raman spectroscopy and X-ray absorption spectroscopy indicate that nitrates are the primary products of this adsorption. Most of these nitrates migrate into the interior of the mordenite and exchange at framework binding sites, returning silver to its unreduced state (AgZ). The remaining nitrates exist at a persistent concentration without aggregating into bulk-phase AgNO 3 . X-ray absorption spectroscopy results further indicate that iodine adsorption occurs on not just Ag 0 Z but also on AgZ and a portion of the nitrates in the system. AgZ adsorbs a sizable quantity of iodine early in the aging process, but its capacity drops rapidly over time. For well-aged samples, nitrates are responsible for up to 95% of mordenite’s iodine capacity. Overall, these results have enhanced our understanding of the aging process in silver mordenite and are expected to guide the development of superior adsorbents for the capture of radioactive iodine from reprocessing off-gas.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Understanding Self-Assembly and the Stabilization of Liquid/Liquid Interfaces: The Importance of Ligand Tail Branching and Oil-Phase Solvation

Organophosphorus-based ligands represent a versatile set of solvent extraction reagents whose chemical makeup plays an important role in extraction mechanism. We hypothesize that the branching of the extractant hydrophobic tail and its oil-phase solvation affect the liquid/liquid interfacial structure. Understanding the structure mediated adsorption and interfacial ordering becomes key in designing ligands with enhanced selectivity and efficiency for targeted extractions. We employed vibrational sum frequency generation spectroscopy and interfacial tension measurements to extract thermodynamic adsorption energies, map interfacial ordering, and rationalize disparate behaviors of model di-(2-ethylhexyl) phosphoric acid and dioctyl phosphoric acid ligands at the hexadecane water interface. With increased surface loading, ligands with branched hydrophobic tails formed stable interfaces at much lower concentrations than those observed for ligands with linear alkyl tails. The lack of an oil phase and associated solvation results in markedly different interfacial properties, and thus measurements made at air/liquid surfaces cannot be assumed to correlate with the processes occurring at buried liquid/liquid interfaces. Here, we attribute these differences in the surface mediated self-assembly to key variations in hydrophobic interactions and tail solvation taking place in the oil phase demonstrating that interactions in both the polar and nonpolar phases are essential to understand self-assembly and function.

36 MATERIALS SCIENCE↗

dynamics of organic-mineral interactions at the metal oxide-solution interface as studied via binding energetics (Final report)

This project focused on addressing longstanding fundamental and experimental uncertainties on how dissolved organic substances (DOS) interact with metal oxide surface under environmentally relevant conditions. By leveraging a custom-built real-time, in-tandem flow adsorption microcalorimetry-UV-Vis/fluorescence spectroscopy platform, we characterized the binding energetics, kinetics and mechanistic pathways driving DOS-metal oxide interactions at temporal resolution on the order of 1-5 seconds. We studied a diverse suite of model organic compounds/substances – including monocarboxylates (e.g. acetate and benzoate), di-carboxylates (oxalate and succinate), amino acids, amino-based nanparticles and natural organic matter – interacting at the mineral-water interface of structurally- and/or chemically distinct metal oxides (including SiO2, boehmite, ferrihydrite, and γ-Al2O3). Our results indicated that DOS-metal oxide interactions are governed by multi-step reaction pathways, often switching between distinct, resolvable enthalpy- and entropy-driven non-electrostatic or electrostatic configurations. To quantify these interactions, we developed and implemented an analytical workflow that integrates peak deconvolution and Monte-Carlo based error propagation to determine site-specific thermodynamic and kinetic parameters for individual binding/debinding events. In addition to resolving apparent first-order rate constants of each event, we were able to quantify associated apparent equilibrium constants as well as free energy, enthalpy and entropy contribution to the activation and subsequent progression of the binding/debinding process across compounds, compound class and metal oxide surfaces. The kinetic-thermodynamic data produced in this study captured how the interplay between oxide surface reactivity and DOS molecular structure jointly drives binding-debinding dynamics. Notably, that at pH below PZC of the oxide surface, neutral species were heavily involved in monocarboxylate binding, while anionic species drove dicarboxylate binding. Also, that among amino acids 1) positional isomers show distinctive binding characteristics to each other while enantiomers show no significant differences in binding characteristics, 2) molecules that bind via outer-sphere complexation show a larger entropic shift between binding and debinding with no impact on oxide surface while 3) inner-sphere interactions increased anion exchange capacity of the oxide surface. The new insights and data from this work has great potential for improving predictive modeling of carbon dynamics and specifically organic-mineral interactions in environmental and industrial systems.

54 ENVIRONMENTAL SCIENCES↗

Dioxygen Activation Kinetics over Distinct Cu Site Types in Cu-Chabazite Zeolites

Cu-exchanged zeolites activate dioxygen to form active sites for partial methane oxidation (PMO), nitrogen oxide decomposition, and carbon monoxide oxidation. Apparent rates of O 2 activation depend both on the intrinsic kinetics of distinct Cu site types and the distributions of such sites within a given zeolite, which depend on the density and arrangement of the framework Al atoms. In this work, we use hydrothermal synthesis methods to control the arrangement of framework Al sites in chabazite (CHA) zeolites and, in turn, the distinct Cu site types formed. Time-resolved in situ Raman spectroscopy reveals the kinetics of O 2 adsorption and activation within these well-defined Cu-CHA materials and the concomitant structural evolution of copper–oxygen (Cu x O y ) complexes, which are interpreted alongside Cu(I) oxidation kinetics extracted from in situ X-ray absorption spectroscopy (XAS). Raman spectra of several plausible Cu x O y species simulated using density functional theory suggest that experimental spectra (λ ex = 532 nm) capture the formation of mono(μ-oxo)dicopper species (ZCuOCuZ). Transient experiments show that the timescales required to form Cu x O y structures that no longer change in Raman spectra correspond to the durations of oxidative treatments that maximize CH 3 OH yields in stoichiometric PMO cycles (approximately 2 h). Yet, these periods extend well beyond the timescales for the complete conversion of the initial Cu(I) intermediates to their Cu(II) states (<0.3 h, reflected in X-ray absorption near edge spectroscopy spectra), which demonstrates that Cu x O y complexes continue to evolve structurally following rapid Cu(I) oxidation. The dependence of ZCuOCuZ formation rates on O 2 pressure, H 2 O pressure, and temperature is consistent with a mechanism in which ZCuOH reduces to form ZCu + sites that bind molecular oxygen and form ZCu-O 2 intermediates. Subsequent reaction with proximate ZCu + forms bridging peroxo dicopper complexes that cleave O–O bonds to form ZCuOCuZ in steps facilitated by water. These data and interpretations provide evidence for the chemical processes that link rapid and kinetically irrelevant Cu oxidation steps (frequently probed by XAS and UV–vis spectroscopy) to the relatively slow genesis of reactive Cu complexes that form CH 3 OH during PMO. In doing so, we reveal previously unrecognized complexities in the processes by which Cu ions in zeolites activate O 2 to form active Cu x O y complexes, which underscore the insight afforded by judicious combinations of experimental and theoretical techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of thermal treatment on structure and catalytic performance of ceria-zirconia supported copper oxide (CuO x /Ce y Zr 1-y O 2 ) catalysts for CO oxidation

Copper oxide (CuO x ) supported on ceria-zirconia (Ce y Zr 1-y O 2 , y = 1.0, 0.5, 0.0) catalysts were investigated to elucidate the effects of thermal treatment on their physicochemical properties and catalytic performance in carbon monoxide (CO) oxidation. Here, the catalysts were synthesized via a one-pot chemical vapor deposition (OP-CVD) method at 700˚C and 900˚C with controlled Cu loading. Characterization techniques, including synchrotron X-ray diffraction (S-XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma spectroscopy (ICP), and N 2 adsorption-desorption, were implemented to probe the crystalline structure, molecular and electronic structure, oxygen vacancies, specific surface area (SSA) and metal loading. CO oxidation was chosen as a model reaction to explore the structure-catalytic performance relationship. A ∼100% CO conversion was achieved at < 150˚C, particularly with the CuO x /CeO 2 catalyst calcined at 700˚C. In contrast, calcination at 900˚C caused a ∼90% decrease in SSA and a ∼24% increase in T 50 . Activity tests revealed that increasing ZrO 2 content lowered CO oxidation activity despite generating more defect sites. In-situ measurement of the 700 °C calcined samples revealed the presence of stable and unstable defects in CuO x /Ce 0.5 Zr 0.5 O 2 and CeO 2 respectively, which play a key role in the activity of the catalysts. The results highlight that catalytic performance is closely related to the SSA. Furthermore, an optimum calcination temperature favor significant oxygen vacancy formation with required CuO x -support interactions, enhancing redox properties and catalytic performance.

36 MATERIALS SCIENCE↗

Disentangling interlayer confinement and pore surface adsorption in functionalized smectites for tunable ethylene gas capture

Smectite-based adsorbents are increasingly being studied as sustainable packaging materials for scavenging ethylene, a plant hormone that accelerates fruit ripening. However, the mechanisms governing their uptake and retention remain poorly understood. Here, to tackle this question we systematically investigate ethylene gas-solid interactions in pristine, acid-activated, and choline-functionalized montmorillonites using a complementary combination of structural, gravimetric, and spectroscopic techniques, including inelastic neutron scattering. We experimentally distinguish ethylene populations associated with interlayer confinement, mesopore, and external surface adsorption. We show that chemical functionalization distinctly controls adsorption pathways: acid activation enhances total uptake by generating mesoporous adsorption sites and promoting partial interlayer intercalation, yielding capacities comparable to those of leading smectite-based adsorbents, while choline functionalization promotes preferential confinement and stabilization of guest molecules within the interlayer galleries. Advanced spectroscopic analysis provides molecular-level insight into confinement environments and interaction strengths. We also establish clear structure-property relationships by correlating uptake values derived from independent techniques, linking chemical modification, accessible adsorption domains, and retention behavior. These findings provide general design principles for tuning gas-solid interactions in functionalized layered silicates and highlight their potential as adaptable platforms for sustainable ethylene gas capture and selective adsorption technologies.

Ethylene adsorption mechanism↗

Novel waste-derived non-noble metal catalysts to accelerate acidic and alkaline hydrogen evolution reaction

Carbon substrate support is a promising approach to facilitate catalytic activity of non-noble metal catalysts in hydrogen evolution reactions (HER). Here, in this paper, we report a waste-derived electrocatalyst P-CoNiO 2 @NC synthesized under mild condition. It exhibits outstanding HER performance in both acid (η 10 = 64.6 mV) and alkaline (η 10 = 96.4 mV) condition with good stability. Especially, it begins to outperform commercial Pt/C when the current density is over 74 mA/cm 2 in acid electrolyte and 29 mA/cm 2 in alkaline electrolyte. Moreover, the waste-derived carbon substrate could effectively promote HER activity of other dual 3d TMOs such as Fe and Co, Fe and Ni. The improved HER activity originates from electron transfer, electronic structure adjustment and optimization of intermediates adsorption according to X -ray photoelectron spectroscopy and density functional theory calculations. This work provides a new insight for converting wastes into value-added products and a sustainable and friendly strategy to facilitate hydrogen energy production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Decoding the Gate Opening Mechanism of the Flexible Framework RPM3–Zn upon Hydrocarbon Inclusion

Although the existence of a gate-opening phenomenon in the flexible RPM3–Zn is well known, the actual mechanism remains a mystery. Here, we provide a full picture that unambiguously identifies and explains the gate-opening mechanism in RPM3–Zn upon exposure to various hydrocarbons—acetylene, ethylene, ethane, propane, and butane—by combining insights gained from calorimetry, adsorption isotherms, PXRD, in situ infrared spectroscopy, and ab initio simulations. We find that the key to gate opening in this framework is the stretching of a bond between an O and the Zn metal center (COO–Zn), acting as a “stabilizer”, which weakens the necessary support required for the structure to remain intact. Consequently, an increasing concentration of guest molecules exerts sufficient internal pressure to induce strong structural transformations in the unit cell shape and volume, thus triggering the gate opening. Here, our results are critical to understanding the gate opening in several other flexible frameworks and provide an opportunity to fine- tune hydrocarbon separation.

36 MATERIALS SCIENCE↗

Improving the performance for direct electrolysis of CO 2 in solid oxide electrolysis cells with a Sr 1.9 Fe 1.5 Mo 0.5 O 6– δ electrode via infiltration of Pr 6 O 11 nanoparticles

Direct CO 2 electrolysis using solid oxide electrolysis cells (CO 2 -SOECs) holds promise to efficiently convert carbon dioxide to carbon monoxide and oxygen. Cathodes with desirable catalytic activity and chemical stability play a critical role in the development of direct CO 2 -SOECs. Although Sr 2 Fe 1.5 Mo 0.5 O 6–δ (SFM) has exhibited promise for direct CO 2 -SOECs due to its redox stability, it suffers from insufficient activity for the CO 2 reduction reaction (CO 2 RR). Here we report interface engineering of nanosized Pr 6 O 11 on the SFM cathode obtained through infiltration to promote the CO 2 RR performance for direct CO 2 -SOECs. The effect of Pr 6 O 11 loading on the performance of the CO 2 RR is systematically investigated. At 800 °C, the current density of the Pr 6 O 11 infiltrated SFM cathode with an optimum Pr 6 O 11 loading of 14.8 wt% reaches 1.61 A cm –2 at 1.5 V, more than double that of the SFM cathode (0.76 A cm –2 ) under the same operating conditions. X-ray photoelectron spectroscopy (XPS) characterization and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) analysis indicate that the adsorption ability of CO 2 on the SFM cathode has been significantly improved by the formation of Pr 6 O 11 . Temperature-programmed desorption (TPD) of CO 2 measurements further manifest that a 14.8 wt% Pr 6 O 11 -SFM cathode has better CO desorption capacity. In addition, polarization resistance of the SFM cathode has significantly decreased with the addition of Pr 6 O 11 . Three-electrode measurement was used to analyze the improved electrode kinetics. Finally, these results demonstrate that the formation of Pr 6 O 11 in the SFM cathode through infiltration is a promising approach for increasing CO 2 RR activity for CO 2 -SOECs.

03 NATURAL GAS↗

A fundamental approach to adhesion: Synthesis, surface analysis, thermodynamics and mechanics

The acid-base properties of titanium 6-4 plates (low surface area) were investigated after three different pretreatments, namely Turco, phosphate-fluoride and Pasa-Jell. A series of indicators was used and color changes were detected using diffuse reflectance visible spectroscopy. Electron spectroscopy for chemical analysis was used to examine the indicator on the Ti 6-4 surface. Specular reflectance infra-red spectroscopy was used to study the adsorption of stearic acid from cyclohexane solutions on the Ti 6-4 surface.

Siriwardane, R.↗

Mechanisms of Zn removal from water by amorphous geopolymer: Molecular-level insights from X-ray absorption spectroscopy, isotope fractionation, and surface complexation modeling

Porous geopolymers have attracted widespread attention as promising heavy metal adsorbents that can be synthesized from aluminosilicate solid wastes. However, the precise microstructural evidence for adsorbed heavy metals on geopolymers remains unclear due to the insensitivity of conventional characterization techniques on minerals with amorphous structure and surface disorder. Batch adsorption and column experiments coupled with X-ray absorption spectroscopy (XAS), Zn stable isotope, and surface complexation model (SCM) were employed to reveal the Zn removal mechanisms with coal fly ash porous geopolymer (CFAPG) at a molecular scale. The macroscopic kinetic and isothermal adsorption of Zn on CFAPG were well described by the pseudo-second-order model and Bi_Langmuir equation, respectively, indicating the presence of abundant heterogeneous active sites on the CFAPG surface. Further, two types of active sites on the CFAPG surface were identified by XAS coupled with Zn isotopes in batch experiments at pH <= 6.0: one is pH-dependent and associated with tetrahedral zinc coordi-nation, and the other is pH-insensitive and associated with octahedral zinc coordination; these sites were confirmed by the bidentate SCM as the variable charge site (surface complexation, >S-OH) and the permanent negative charge site (cation exchange, >X - ), respectively. Furthermore, the important contribution of surface co -precipitation besides surface complexation and cation exchange to the Zn adsorption on CFAPG was identified by XAS coupled with SCM in a flow-through column experiment at pH >6.0. These investigations provide a systemic understanding of the Zn adsorption mechanisms on CFAPG and an SCM reference for the application and prediction of geopolymers in heavy metal-contaminated water remediations.

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