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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 775 records · Page 43
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Perrhenate incorporation into binary mixed sodalites: The role of anion size and implications for technetium-99 sequestration

Perrhenate (ReO 4 - ), as a TcO 4 - analogue, was incorporated into mixed-anion sodalites from binary solutions containing ReO 4 - and a competing anion X n- (Cl - , CO 3 2- , SO 4 2- , MnO 4 - , or WO 4 2- ). For this study, our objective was to determine the extent of solid solution formation and the dependence of competing ion selectivity on ion size. Using equivalent aqueous concentrations of the anions (ReO 4 - /X n- molar ratio = 1:1), we synthesized mixed-anion sodalites from zeolite and NaOH at 90 °C for 96 h. The resulting solids were characterized by bulk chemical analysis, powder X-ray diffraction, scanning electron microscopy, and X-ray absorption near edge structure (XANES) spectroscopy to determine crystal structure, chemical composition, morphology, and rhenium (Re) oxidation state. Rhenium in the solid phase occurred predominately as Re(VII)O 4 - in the sodalites, which have a primitive cubic pattern in the space group P43n. The refined unit-cell parameters of the mixed sodalites ranged from 8.88 to 9.15 Å and showed a linear dependence on the size and mole fraction of the incorporated anion(s). The ReO 4 - selectivity, represented by its distribution coefficient (K d ), increased in the following order: Cl - < NO 3 - < MnO 4 - and CO 3 2- < SO 4 2- < WO 4 2- for the monovalent and divalent anions, respectively. The relationship between the ReO 4 - distribution coefficient and competing anion size was nonlinear. When the difference in ionic radius (DIR) between ReO 4 - and X n - (n = 1 or 2) was greater than ~ 12%, then ReO 4 - incorporation into sodalite was insignificant. The results imply that anion size is the major factor that determines sodalite anion compositions. Given the similarity in chemical behavior and anion size, ReO 4 - serves as a suitable analogue for TcO 4 - under oxidizing conditions where both elements are expected to remain as oxyanions in the + 7 oxidation state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Effect of particle size on the capture of uranium oxide colloidal particles from aqueous suspensions via high-gradient magnetic filtration

The effectiveness of High Gradient Magnetic Filtration (HGMF) in capturing uranium oxide particles from suspensions was investigated in this study. Two sets of experiments were performed to evaluate the importance of size on the capture of uranium oxide particles. The first considered two batches sieved into size bins of< 5, 5–10, 10–15, and 15–20 µm, while the second was performed using two suspensions with diameters smaller than 1.0 µm and between 1.0 and 1.5 µm. Iron oxide experiments, with particles between 0.3 and 0.8 µm, were performed for calibration purposes. In all experiments, a surfactant (Triton-X100 or sodium dodecyl sulfate) was used to prevent particle aggregation and limit the influence of non-magnetic capture mechanisms. A magnetic field of approximately 1.1 Tesla was generated using a water cooled electromagnet. HGMF was performed using tubular filters packed with ferromagnetic stainless-steel wool. Of the initial four uranium oxide particle sizes, magnetic capture was only observed for particles with a diameter of less than 5 µm, while larger particles experienced no magnetic and minimal total capture. For particles with diameters smaller than 1.0 µm and between 1.0 and 1.5 µm, capture efficiencies increased by 39 ± 9% and 34 ± 6% respectively, solely due to the magnetic field. Although the magnetic force is proportional to particle diameter, the capture efficiency decreased as diameter increased. So these results suggest that Brownian diffusion, which is influential for micron sized particles and increases with decreasing particle size, is acting in conjunction with the magnetic force to influence the efficacy of HGMF for uranium oxide. This important finding underscores the effectiveness of Brownian diffusion in increasing the rate of collision between particles and collector fibers. A stochastic trajectory model was developed to incorporate the influence of Brownian motion on particle behavior and filter removal efficiency. Modeling results are discussed and compared for uranium and iron oxide particles.

42 ENGINEERING↗
DOE OSTI2015

Size-segregated emissions and metal content of vehicle-emitted particles as a function of mileage: Implications to population exposure

The study aims at investigating the characteristics (size distribution, active surface and metal content) of particles emitted by cars as a function of mileage using a novel methodology for characterizing particulate emissions captured by Exhaust Gas Suspension (EGS). EGS was obtained by passing the exhaust gases through a container of deionized water. EGS analysis was performed using laser granulometry, electron scanning microscopy, and high resolution mass spectrometry. Implications of the differences in key features of the emitted particles on population exposure were investigated using numerical simulation for estimating size-segregated PM deposition across human respiratory tract (HRT). It was found that vehicle mileage, age and the respective emissions class have almost no effect on the size distribution of the exhaust gas particulate released into the environment; about half of the examined vehicles with low mileage were found to release particles of aerodynamic diameter above 10 μm. The exhaust gas particulate detected in the EGS of all cars can be classified into three major size classes: (1) 0.1–5 µm – soot and ash particles, metals (Au, Pt, Pd, Ir); (2) 10–30 µm – metal (Cr, Fe, Cu, Zr, Ni) and ash particles; (3) 400–1,000 µm – metal (Fe, Cr, Pb) and ash particles. Newer vehicles with low mileage are substantial sources of soot and metal particles with median diameter of 200 nm with a higher surface area (up to 89,871.16 cm{sup 2}/cm{sup 3}). These tend to deposit in the lower part of the human respiratory tract. - Highlights: • Car mileage has virtually no effect on the size of the solid particles released. • Newer diesel vehicles emit particles of lower aerodynamic diameter. • Particle active surface emitted by newer vehicles is on average 3 times higher. • Real-life emissions were translated into actual internal PM exposure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Tailoring Cu-Zr gradient nanoglass structures: Influence of nanoparticle size and cooling rates on glass-glass interfaces

The study of gradient nanoglasses (GNGs) has gained attention due to their unique mechanical properties and potential applications in advanced materials. This study employs molecular dynamics simulations to synthesize a GNG using Cu-Zr metallic glass nanoparticles (NPs) sized from 3 to 15 nm. The NPs were produced by melting and quenching metallic clusters at a relatively slow quench rate of 10 9 K/s. The synthesis of GNG is elucidated along with the characterization of its heterogeneous metallic glass nanostructure. A seamless GNG structure is formed through cold compression of Cu 64 Zr 36 amorphous NPs of varying sizes. The influence of NP size on the GNG structure is investigated, utilizing deeply relaxed NPs, which exhibit a characteristic Cu segregation pattern on their surfaces. The results highlight an increase in structural heterogeneity due to heterogeneous mass transport and the development of local composition and density variations caused by Cu segregation at glass-glass interfaces (GGIs). A reduction in NP size is correlated with decreased Cu atomic displacements and local density at GGIs, suggesting that larger NPs may produce stronger GGIs. This research presents a novel methodology for synthesizing heterogeneous metallic glasses, demonstrating the capacity to control and customize nanostructure heterogeneity through the manipulation of NP sizes and cooling rates. Furthermore, these findings enhance our understanding of structural evolution during nanoglass synthesis and lay the foundation for further exploration in nanomaterial synthesis and characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Exploring the relationship between solvent-assisted ball milling, particle size, and sintering temperature in garnet-type solid electrolytes

Garnet-type solid electrolytes, such as Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO), are promising materials for solid-state batteries, but processing remains a challenge, in part due to the high sintering temperature required for densification. Additionally, this temperature can be lowered by decreasing the initial particle size via solvent-assisted ball milling, but the relationship between solvent choice, particle properties, sintering behavior, and ionic conductivity is not well understood. In this work, we systematically explore these parameters, showing that milling in commonly used protic solvents, such as alcohols, effectively decreases the particle size but results in lithium loss (through Li + /H + exchange) that leads to poor sintering. By contrast, milling in aprotic solvents with surfactant reduces the particle size to ~220 nm without lithium loss, enabling the fabrication of dense samples (5.1 g/cm 3 ) with good ionic conductivity (0.43 mS/cm at 25 °C) at a lower sintering temperature (1000 °C). We compare ionic conductivities and activation energies for samples prepared with different particle sizes and sintering temperatures and use multiphase-field simulations to identify the mass transport and microstructural mechanisms responsible for the observed sintering dependence on particle size. These results further clarify the relationship between processing parameters and performance and represent important progress toward overcoming fabrication challenges for these materials.

25 ENERGY STORAGE↗
DOE OSTI2014

Optical phonons in nanostructured thin films composed by zincblende zinc selenide quantum dots in strong size-quantization regime: Competition between phonon confinement and strain-related effects

Raman scattering in combination with optical spectroscopy and structural studies by X-ray diffraction was employed to investigate the phonon confinement and strain-induced effects in 3D assemblies of variable-size zincblende ZnSe quantum dots close packed in thin film form. Nanostructured thin films were synthesized by colloidal chemical approach, while tuning of the nanocrystal size was enabled by post-deposition thermal annealing treatment. In-depth insights into the factors governing the observed trends of the position and half-width of the 1LO band as a function of the average QD size were gained. The overall shifts in the position of 1LO band were found to result from an intricate compromise between the influence of phonon confinement and lattice strain-induced effects. Both contributions were quantitatively and exactly modeled. Accurate assignments of the bands due to surface optical (SO) modes as well as of the theoretically forbidden transverse optical (TO) modes were provided, on the basis of reliable physical models (such as the dielectric continuum model of Ruppin and Englman). The size-dependence of the ratio of intensities of the TO and LO modes was studied and discussed as well. Relaxation time characterizing the phonon decay processes in as-deposited samples was found to be approximately 0.38 ps, while upon post-deposition annealing already at 200 °C it increases to about 0.50 ps. Both of these values are, however, significantly smaller than those characteristic for a macrocrystalline ZnSe sample. - Graphical abstract: Optical phonons in nanostructured thin films composed by zincblende zinc selenide quantum dots in strong size-quantization regime: competition between phonon confinement and strain-related effects. - Highlights: • Phonon confinement vs. strain-induced effects in ZnSe 3D QD assemblies were studied. • Shifts of the 1LO band result from an intricate compromise between the two effects. • SO and theoretically forbidden TO modes were accurately assigned. • Phonon relaxation time in as-deposited and annealed samples is 0.38 ps and 0.50 ps. • Both values are significantly smaller than in macrocrystalline ZnSe sample.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Influence of porous aluminosilicate grain size materials in experimental and modelling Cs + adsorption kinetics and wastewater column process

This paper focuses on the influence of the grain size of a geopolymer based adsorbent on its Cs + adsorption performances both in batch and fixed-bed process. The geopolymer phase was used as a binder to support NaY zeolite particle in a 20 wt% charged porous composite with 160 m 2 .g –1 of porous surface area. These samples were shaped with three grain sizes (50 /100/500 µm) to remove 80–90 mg/g of Cs + in batch and column operations. After their microstructural and porous characterizations, their efficiency and adsorption characteristics were investigated through adsorption isotherms and kinetic in the two processes. While the grain size has no influence on the maximal extraction capacity of the adsorbent, it strongly affects the sorption kinetic. By coupling experimental data and a modelling approach, the complex sorption mechanism was highlighted, suggesting a new insight of the contaminant sorption kinetic. Then, comparison of batch and column adsorption experiments illustrates the detailed explanation of various process parameters for column study. The results show challenges for fixed-bed column utilization by the choice of the appropriate grain size as a compromise between the material sorption kinetic and hydrodynamic considerations. Furthermore, this is of high importance to more accurately optimize the design of column adsorption to assess the transport of Cs+ in multi-porous tailored grain size materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Impact of mixed grain size sediment input on braided river Morphodynamics: Insights from experimental and numerical modeling

The rate of sediment supply has significant impacts on river morphology, making it crucial to understand the geomorphic changes and grain size distribution dynamics in rivers. However, the effects of varying grain size sediment input on morphological changes in braided channels remain poorly understood. This study is the first to investigate the bar development and sediment sorting processes in braided channels with non-uniform sediment inputs using both numerical and experimental approaches. We applied a two-dimensional numerical model, Nays2DH to confirm and generalize experimental results. The model reproduced key experiment results, including 1) stream elevation changes, and 2) grain size distribution. Using this validated model, we explored the morphological changes and sorting process in a braided river with sediment inputs. The numerical experiments demonstrate that sediment input controls the elevation of the stream bed and the grain size distribution. Notably, both the elevation and grain-size distribution become relatively stable in downstream of the channel. Additionally, the simulation results suggest that an increased sediment supply leads to greater channel complexity, with bed surface armoring decreasing.

Nays2DH↗
DOE OSTI2015

Effects of combined silicon and molybdenum alloying on the size and evolution of microalloy precipitates in HSLA steels containing niobium and titanium

The effects of combined silicon and molybdenum alloying additions on microalloy precipitate formation in austenite after single- and double-step deformations below the austenite no-recrystallization temperature were examined in high-strength low-alloy (HSLA) steels microalloyed with titanium and niobium. The precipitation sequence in austenite was evaluated following an interrupted thermomechanical processing simulation using transmission electron microscopy. Large (~ 105 nm), cuboidal titanium-rich nitride precipitates showed no evolution in size during reheating and simulated thermomechanical processing. The average size and size distribution of these precipitates were also not affected by the combined silicon and molybdenum additions or by deformation. Relatively fine (< 20 nm), irregular-shaped niobium-rich carbonitride precipitates formed in austenite during isothermal holding at 1173 K. Based upon analysis that incorporated precipitate growth and coarsening models, the combined silicon and molybdenum additions were considered to increase the diffusivity of niobium in austenite by over 30% and result in coarser precipitates at 1173 K compared to the lower alloyed steel. Deformation decreased the size of the niobium-rich carbonitride precipitates that formed in austenite. - Highlights: • We examine combined Si and Mo additions on microalloy precipitation in austenite. • Precipitate size tends to decrease with increasing deformation steps. • Combined Si and Mo alloying additions increase the diffusivity of Nb in austenite.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The effect of cell-size dispersity on the mechanical properties of closed-cell aluminum foam

Highlights: • The effect of cell-size dispersity on the Young’s modulus of foam was investigated through experiments and simulations • Crushing experiments were conducted on 27 foam specimens in order measure the relative Young’s modulus • Three types of numerical models, including monodispersed, bidispersed and polydispersed models were studied • The numerical convergence on the model size for different models was also studied • The difference among numerical results obtained from the three models was insignificant - Abstract: The mechanical properties of open-celled and closed-celled metallic foam are strongly influenced by the cellular microstructure and material properties of the base material from which the foam is made. The present study investigated the microstructure and mechanical properties of ALPORAS closed-cell Al foam. In particular, the effect of cell-size dispersity on the Young's modulus of foam was investigated through crushing experiments and numerical simulations. Crushing experiments were first conducted on two mutually perpendicular directions. Numerical models of varying cell-size dispersity and complexity were subsequently developed, including the monodispersed model that is based on the Kelvin structure, the bidispersed model, and the polydispersed model that is based on the random Laguerre tessellation algorithm. The numerical models were discretized using shell elements, and the simulations were conducted using the ABAQUS finite element method software. Relative Young's moduli with various relative densities were predicted, and the numerical convergence on the model size was studied accordingly. Numerical results obtained from all three numerical models developed were found to overestimate the experimental results by a factor of approximately 3. The difference between the numerical and experimental results can be attributed to the difference in detailed microstructural characteristics. Furthermore, the difference among numerical results obtained from the three models was insignificant.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Dynamic recrystallization of a wrought magnesium alloy: Grain size and texture maps and their application for mechanical behavior predictions

Effect of dynamic recrystallization (DRX) on the grain refinement and texture modification was studied by conducting a series of hot compression on AZ31B Mg alloy. Processing-grain size-texture maps were established as a function of temperature, strain rate, strain, and the Zener-Hollomon parameter (Z). Moreover, influence of simultaneous changes in the grain size and texture on tensile yield strength and ductility of the hot-worked Mg alloy was studied using the grain size and texture maps established. The processing-grain size map showed that the DRX grain size decreased with the increase in Z, also revealing various characteristics ranging from a grain growth, grain refinement, to a bimodal distribution of ultrafine grains and partially recrystallized grains. The effect of twinning on the grain refinement was also evident at high Z conditions. The processing-texture map revealed that the initial fiber texture was altered significantly to a shear, off-normal, or extension-twin texture with the increase in Z. The Schmid-factor maps were calculated to identify a dominant deformation mode during a subsequent tensile deformation of the hot-worked samples. Finally, a corresponding Hall-Petch relationship for each dominant deformation mode was used to establish tensile yield-strength maps, which agree well with the measured data.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Size effect on electronic transport in nC–Si/SiO{sub x} core/shell quantum dots

Highlights: ► Electrical conductivity (σ) demonstrated to exhibit quantum size effect for Si-QDs. ► High σ ∼ 4 × 10{sup −2} S cm{sup −1} for Si-QDs of average size ∼3.7 nm, number density ∼4.8 × 10{sup 11} cm{sup −2}. ► Heterojunction-like band-structure at the QD interface controls electronic transport. -- Abstract: Electronic transport in silicon quantum dots (Si-QDs) in core/shell configuration was studied. The nC–Si cores encapsulated by protective SiO{sub x} shells embedded in a-Si matrix were obtained from one-step and spontaneous plasma processing, at low substrate temperature (300 °C) compatible for device fabrication. The size, density and distribution of nC–Si QDs were controlled by optimizing the plasma parameters. Very high electrical conductivity, σ ∼ 4 × 10{sup −2} S cm{sup −1}, was achieved at a total number density of Si-QDs, N ∼ 4.8 × 10{sup 11} cm{sup −2}, corresponding to the lowering in its average core size, d ∼ 3.7 nm, to the order of the bulk Si exciton Bohr radius and the associated quantum confinement effects. The electrical conductivity was demonstrated to exhibit quantum size (3 < d (nm) < 10) effect in zero dimensional quantum dots. The underlying electronic transport was explained using heteroquantum-dot model, the nC–SiO{sub x}:H QDs possess hetero-junction like band structure in the interface regions, due to their different band gaps.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Size-controllable porous NiO electrodes for high-performance lithium ion battery anodes

Highlights: • Size-controllable porous NiO electrodes were prepared by a simple thermal oxidation route. • The prepared porous NiO electrodes exhibit high capacity and excellent rate capability and cycling stability. • The smaller nanopore and crystallite size are benefical to improve the electrochemical properties of the porous NiO electrodes. - Abstract: Size-controllable porous NiO electrodes were prepared by a simple and easily scalable thermal oxidation route and were evaluated as anode materials for lithium ion batteries. The nanopore size of the prepared electrodes can be obtained in the range from 20 to 80 nm by varying the thermal oxidation condition. Lithium storage performance measurement showed that porous NiO electrodes exhibit high capacity and excellent rate capability and cycling stability. Furthermore, it was shown that the smaller nanopore and crystallite size are beneficial to improve the electrochemical properties of the porous NiO electrodes.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Grain-size dependent mechanical behavior of nanocrystalline metals

Grain size has a profound effect on the mechanical response of metals. Molecular dynamics continues to expand its range from a handful of atoms to grain sizes up to 50 nm, albeit commonly at strain rates generally upwards of 10 6 s -1 . In this work, we examine the most important theories of grain size dependent mechanical behavior pertaining to the nanocrystalline regime. For the sake of clarity, grain sizes d are commonly divided into three regimes: d>1 μm, 1 μm < d < 100 nm; and d<100 nm. These different regimes are dominated by different mechanisms of plastic flow initiation. We focus here in the region d<100 nm, aptly named the nanocrystalline region. An interesting and representative phenomenon at this reduced spatial scale is the inverse Hall–Petch effect observed experimentally and in MD simulations in FCC, BCC, and HCP metals. Significantly, we compare the results of molecular dynamics simulations with analytical models and mechanisms based on the contributions of Conrad and Narayan and Argon and Yip, who attribute the inverse Hall–Petch relationship to the increased contribution of grain-boundary shear as the grain size is reduced. The occurrence of twinning, more prevalent at the high strain rates enabled by shock compression, is evaluated.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Size effect on the growth and pulverization behavior of Si nanodomains in SiO anode

Silicon monoxide (SiO) as a promising silicon-based anode electrode of lithium-ion batteries (LIBs) has been the subject of many recent investigations. However, the complex microstructural features of SiO hinder attempts to link the microstructure changes in SiO with its electrochemical performances upon electrochemical cycling. This study employs X-ray pair distribution function (PDF), with a high-resolution transmission electron microscope (HRTEM), to investigate the microstructure of Si nanodomains in SiO and its structural evolution over the electrochemical cycling process. The experiment results reveal the size evolution of Si nanodomains in SiO during the electrochemical cycling and find it highly dependent on the initial Si domain size in SiO. If the initial Si domain size is too large, the average size of Si nanodomains would increase at first and then decrease after a certain number of cycles, which indicates the pulverization of Si domains after the electrochemical-driven growth of Si nanodomains reaches a critical point. Furthermore, these results suggest that an optimal initial Si nanodomain size of 4-6 nm for SiO anode materials is essential to retard the growth and subsequent pulverization process of Si nanodomains and thus to improve the cyclability of SiO during long-term cycling.

25 ENERGY STORAGE↗
DOE OSTI2026

Heliostat sizing methodology for concentrating solar thermal industrial process heat projects

This study presents a method to obtain a heliostat size that minimizes the levelized cost of heat (LCOH) of a heliostat-based concentrating solar thermal system for applications of solar heating for industrial processes at operating temperatures from 565 to 1550°C. The method extends prior work by embedding a routine for system design that obtains near-optimal subsystem sizes, increasing the fidelity of drive cost functions, and adding an optical performance model to supplement the previously developed cost models, which we update to reflect current pricing trends. An illustrative business case is developed for Daggett, California, targeting specified annual thermal energy outputs of 50 to 400 GWh th . Optical performance is modeled using verified estimates from the literature. A surrogate heliostat cost model, derived from commercial heliostat designs and scaled for production volume, installation, and operations and maintenance costs, is used to develop cost functions. Results show that heliostat size strongly affects the LCOH, producing a characteristic U-shaped trend with a robust near-optimal window of 7-20 m 2 ; the heliostat size producing the lowest project cost in our study grows slightly as the project size increases, and is reduced as the operating temperature increases. The findings in this study are consistent with the general trend of smaller heliostats being deployed at existing projects for high-temperature industrial process heat and reflect the significant reduction in power electronics and other per-heliostat costs. The methodology we propose is general and can be tailored to revised cost curves as the technology continues to evolve.

14 SOLAR ENERGY↗
DOE OSTI2013

Effect of myonuclear number and mitochondrial fusion on Drosophila indirect flight muscle organization and size

Mechanisms involved in establishing the organization and numbers of fibres in a muscle are not completely understood. During Drosophila indirect flight muscle (IFM) formation, muscle growth is achieved by both incorporating hundreds of nuclei, and hypertrophy. As a result, IFMs provide a good model with which to understand the mechanisms that govern overall muscle organization and growth. We present a detailed analysis of the organization of dorsal longitudinal muscles (DLMs), a subset of the IFMs. We show that each DLM is similar to a vertebrate fascicle and consists of multiple muscle fibres. However, increased fascicle size does not necessarily change the number of constituent fibres, but does increase the number of myofibrils packed within the fibres. We also find that altering the number of myoblasts available for fusion changes DLM fascicle size and fibres are loosely packed with myofibrils. Additionally, we show that knock down of genes required for mitochondrial fusion causes a severe reduction in the size of DLM fascicles and fibres. Our results establish the organization levels of DLMs and highlight the importance of the appropriate number of nuclei and mitochondrial fusion in determining the overall organization, growth and size of DLMs. - Highlights: • Drosophila dorsal longitudinal muscles are similar to vertebrate skeletal muscles. • A threshold number of myoblasts governs the organization of a fibre and its size. • Mitochondrial fusion defect leads to abnormal fibre growth and organization.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2015

CaCO 3 Crystallite Evolution during CaO Carbonation: Critical Crystallite Size and Rate Constant Measurement by In-Situ Synchrotron Radiation X-ray Powder Diffraction

In this work, the evolution of the CaCO 3 crystalline phase during the CaO–CO 2 reaction was investigated by means of in situ synchrotron radiation X-ray powder diffraction performed at the Advanced Photon Source (APS) facilities of the Argonne National Laboratory. CO 2 absorption experiments were carried out in a high temperature reaction capillary with a controlled atmosphere of pure carbon dioxide (CO 2 partial pressure of 1 bar) and in the temperature range between 450 and 750 °C, using CaO-based sorbents obtained by calcination of commercial calcium carbonate. The Rietveld refinement method was applied to estimate the average size of the CaCO 3 crystallites formed during a carbonation time of 20 min, as a function of the carbonation temperature and of the initial calcination conditions. Local maxima were observed in the CaCO 3 crystallite size versus time curves and were identified as the critical CaCO 3 crystallite sizes, marking the transition between the first fast carbonation stage and the second reaction stage controlled by product-layer diffusion. A relationship between this parameter and the reaction temperature, as well as with the initial (at the beginning of carbonation) CaO crystallite size, were found. The CaCO 3 critical crystallite sizes were used to estimate the active surface areas of the CaO sorbent particles where CaCO 3 crystals form and grow. Here, the computed active surface areas were utilized to calculate the kinetic parameters of the surface carbonation reaction: a reaction rate constant of 4.41 × 10 –4 mol/m 2 s, with zero-activation energy, was obtained.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗