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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 901 records · Page 50
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Microstructure investigations of Yb- and Bi-doped Mg{sub 2}Si prepared from metal hydrides for thermoelectric applications

Within the field of thermoelectric materials for energy conversion magnesium silicide, Mg{sub 2}Si, is an outstanding candidate due to its low density, abundant constituents and low toxicity. However electronic and thermal tuning of the material is a required necessity to improve its Figure of Merit, zT. Doping of Yb via reactive YbH{sub 2} into the structure is performed with the goal of reducing the thermal conductivity. Hydrogen is released as a by-product at high temperatures allowing for facile incorporation of Yb into the structure. We report on the properties of Yb- and Bi-doped Mg{sub 2}Si prepared with MgH{sub 2} and YbH{sub 2} with the focus on the synthetic conditions, and samples’ microstructure, investigated by various electron microscopy techniques. Yb is found in the form of both Yb{sub 3}Si{sub 5} inclusions and Yb dopant segregated at the grain boundary substituting for Mg. The addition of 1 at% Yb concentration reduced the thermal conductivity, providing a value of 30 mW/cm K at 800 K. In order to adjust carrier concentration, the sample is additionally doped with Bi. The impact of the microstructure on the transport properties of the obtained material is studied. Idealy, the reduction of the thermal conductivity is achieved by doping with Yb and the electronic transport is adjusted by doping with Bi. Large grain microstructure facilitates the electronic transport. However, the synthetic conditions that provide the optimized microstructure for electrical transport do not facilitate the additional Yb dopant incorporation. Therefore, the Yb and Bi containing sample with the optimized microstructure provides a zT=0.46 at 800 K. - Graphical abstract: 1% or less addition of YbH{sub 2} to Mg{sub 2}Si significantly reduces the thermal conductivity of the material. Yb replaces some Mg in Mg{sub 2}Si and the remainder is distributed as Yb{sub 3}Sb{sub 5} in the Yb-doped Mg{sub 2}Si matrix. Correlation between the observed grain size and transport show the difficulty in simultaneously reducing the thermal conductivity with optimal electronic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Mining the human urine proteome for monitoring renal transplant injury

The human urinary proteome reflects systemic and inherent renal injury perturbations and can be analyzed to harness specific biomarkers for different kidney transplant injury states. 396 unique urine samples were collected contemporaneously with an allograft biopsy from 396 unique kidney transplant recipients. Centralized, blinded histology on the graft was used to classify matched urine samples into categories of acute rejection (AR), chronic allograft nephropathy (CAN), BK virus nephritis (BKVN), and stable graft (STA). Liquid chromatography–mass spectrometry (LC-MS) based proteomics using iTRAQ based discovery (n=108) and global label-free LC-MS analyses of individual samples (n=137) for quantitative proteome assessment were used in the discovery step. Selected reaction monitoring (SRM) was applied to identify and validate minimal urine protein/peptide biomarkers to accurately segregate organ injury causation and pathology on unique urine samples (n=151). A total of 958 proteins were initially quantified by iTRAQ, 87% of which were also identified among 1574 urine proteins detected in LC-MS validation. 103 urine proteins were significantly (p<0.05) perturbed in injury and enriched for humoral immunity, complement activation, and lymphocyte trafficking. A set of 131 peptides corresponding to 78 proteins were assessed by SRM for their significance in an independent sample cohort. A minimal set of 35 peptides mapping to 33 proteins, were modeled to segregate different injury groups (AUC =93% for AR, 99% for CAN, 83% for BKVN). Urinary proteome discovery and targeted validation identified urine protein fingerprints for non-invasive differentiation of kidney transplant injuries, thus opening the door for personalized immune risk assessment and therapy.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2013

Microstructural, mechanical and weldability assessments of the dissimilar welds between γ′- and γ″-strengthened nickel-base superalloys

Dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys has been investigated to identify the relationship between the microstructure of the welds and the resultant mechanical and weldability characteristics. γ′-Strengthened nickel-base Alloy 500 and γ″-strengthened nickel-base Alloy 718 were used for dissimilar welding. Gas tungsten arc welding operations were utilized for performing the autogenous dissimilar welding. Alloy 500 and Alloy 718 base metals showed various types of phases, carbides, intermetallics and eutectics in their microstructure. The results for Alloy 500 weld metal showed severe segregation of titanium to the interdendritic regions. The Alloy 718 weld metal compositional analysis confirmed the substantial role of Nb in the formation of low-melting eutectic-type morphologies which can reduce the weldability. The microstructure of dissimilar weld metal with dilution level of 65% wt.% displayed semi-developed dendritic structure. The less segregation and less formation of low-melting eutectic structures caused to less susceptibility of the dissimilar weld metal to the solidification cracking. This result was confirmed by analytic modeling achievements. Dissolution of γ″-Ni{sub 3}Nb precipitations took place in the Alloy 718 heat-affected zone leading to sharp decline of the microhardness in this region. Remelted and resolidified regions were observed in the partially-melted zone of Alloy 500 and Alloy 718. Nevertheless, no solidification and liquation cracking happened in the dissimilar welds. Finally, this was concluded that dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys can successfully be performed. - Highlights: • Dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys is studied. • Microstructural, mechanical and weldability aspects of the welds are assessed. • Microstructure of welds, bases and heat-affected zones is characterized in detail. • The type, morphology and distribution of the phases are thoroughly investigated. • Dissimilar welding is successfully performed without occurrence of any hot cracks.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Effect of re-melting on particle distribution and interface formation in SiC reinforced 2124Al matrix composite

The interface between metal matrix and ceramic reinforcement particles plays an important role in improving properties of the metal matrix composites. Hence, it is important to find out the interface structure of composite after re-melting. In the present investigation, the 2124Al matrix with 10 wt.% SiC particle reinforced composite was re-melted at 800 °C and 900 °C for 10 min followed by pouring into a permanent mould. The microstructures reveal that the SiC particles are distributed throughout the Al-matrix. The volume fraction of SiC particles varies from top to bottom of the composite plate and the difference increases with the decrease of re-melting temperature. The interfacial structure of re-melted 2124Al–10 wt.%SiC composite was investigated using scanning electron microscopy, an electron probe micro-analyzer, a scanning transmission electron detector fitted with scanning electron microscopy and an X-ray energy dispersive spectrometer. It is found that a thick layer of reaction product is formed at the interface of composite after re-melting. The experimental results show that the reaction products at the interface are associated with high concentration of Cu, Mg, Si and C. At re-melting temperature, liquid Al reacts with SiC to form Al{sub 4}C{sub 3} and Al–Si eutectic phase or elemental Si at the interface. High concentration of Si at the interface indicates that SiC is dissociated during re-melting. The X-ray energy dispersive spectrometer analyses confirm that Mg- and Cu-enrich phases are formed at the interface region. The Mg is segregated at the interface region and formed MgAl{sub 2}O{sub 4} in the presence of oxygen. The several elements identified at the interface region indicate that different types of interfaces are formed in between Al matrix and SiC particles. The Al–Si eutectic phase is formed around SiC particles during re-melting which restricts the SiC dissolution. - Highlights: • Re-melted composite shows homogeneous particle distribution • Thick reaction products are observed at the interface • Carbide is identified at interface due to SiC dissolution at high temperature • Reaction products are also Si enrich phase • Mg and Cu segregated and formed MgAl{sub 2}O{sub 4}, CuMgAl{sub 2} phase at grain boundary.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Feasibility of formation of nanocrystalline Fe-Cr-Y alloys: Mechanical properties and thermal stability

Aim of the present study is to investigate the feasibility of formation of Fe-Cr-Y disordered solid solutions by mechanical alloying and effect of Y on the thermal stability and mechanical properties of such nanocrystalline alloys. Thermodynamic analysis by Miedema's and Toop's models confirms that the energy barrier required to form the disordered solid solutions has been overcome by the stored energy due to strain dislocations and grain boundary defects. Although limited grain growth was observed during annealing of metastable Fe-15Cr-1Y alloy, the grains size found to stabilize at ~ 53 nm after annealing at 1000 °C; and the corresponding hardness value measured to be also quite high (8 GPa). The grain size analysis by TEM and AFM is well-corroborated with the XRD crystallite size. The high thermal stability and large strengthening effect have been discussed in the light of grain boundary pinning by solute segregation, solute drag effect and Zener pinning due to intermetallic phase(s). - Highlights: • Metastable Fe-Cr-Y alloys were developed by mechanical alloying for nuclear applications. • Formation of Fe-Cr-Y solid solutions was explained from the Gibbs free energy change using Toop's model. • 1 at.% Y found to be very effective in the stabilization of Fe-Cr alloys at high temperatures. • Solute drag effect and/or segregation of Y atoms played a pivotal role in the stabilization.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Ghost microstructure evolution and identification in the coarse grain heat affected zone of 2.25Cr-1Mo-V-Ti steel using tint etching

Microstructural characteristics of the CGHAZ (coarse grained heat affected zone) made of the 2.25Cr-1Mo-V-Ti material for the thermal power plant boiler tube were discussed using the technique of tint etching. To conduct the micro structural characterization, the sample on which CGHAZ was produced by using a high temperature thermal cycle simulator, Gleeble 3500 equipment was used for comparative analyses using the existing Nital etching (ASTM E407-74) and the alkaline etching (ASTM E40785). The latter was used to observe a specific phase. For the microstructure on which the alkaline etching was experimented, the shape of a black strip (Ghost microstructure) in a few microns was observed, which was not observed from the Nital etching. It was found from the phase identifications based EPMA, EBSD and TEM experiments that the image of the black strip in a few microns represented the alpha phase in which C, Cr and Mo became segregated. In addition, it was verified that austenite and M{sub 23}C{sub 6} phase were present around the segregated zone. Based on such results, the mechanism by which the image of the black strip in a few microns was formed at the CGHAZ. In this study, we have investigated the mechanism of the appeared black strip in the CGHAZ. - Highlights: •Ghost microstructure was observed which was not observed from the nital etching. •Ghost microstructure has high concentrations of carbon and molybdenum than matrix. •Schematic illustration proposed of why Ghost microstructure was generated. •Ghost microstructure caused by partial dissolution of M{sub 23}C{sub 6} precipitation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The evolution history of superalloy powders during hot consolidation and plastic deformation

Highlights: • Element segregations in a powder metallurgy superalloy at different states are identified. • The surface energy drives precipitation of oxides, carbides, and γ' particles on powder surface during hot consolidation. • Prior particle boundary structure is distorted and more uniformly refined grains are obtained after hot extrusion. - Abstract: Powder metallurgy superalloys are widely used to produce critical rotating parts in turbine engines. However, the issues like what is the driving force of precipitation on prior particle boundary (PPB) during consolidation and how the PPB structure evolves during plastic deformation still remain to be resolved. In this study, with the characterization of the microstructure evolution from powder, consolidation, to plastic deformation, the segregation of alloying elements on the particle boundaries at elevated temperature was analyzed by equilibrium thermodynamic calculations, and the distortion of PPB structure under large plastic deformation was quantitively simulated by finite element (FE) methods. The results indicated that surface energy serves as the main driving force of PPB precipitation and hot extrusion could distort the PPB structure and yield more uniformly refined grains.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Advanced 3D characterisation of iodine induced stress corrosion cracks in zirconium alloys

Highlights: • Macroscopic crack direction is affected by metallurgical state. • High resolution XCT reveals complex crack morphology. • 3D-EBSD used to fully characterise attacked grain boundaries. • Evidence of iodine segregation ahead of a crack tip. - Abstract: In this study, a range of advanced techniques have been used to characterise iodine-induced stress corrosion cracks, and investigate their interaction with microstructure in zirconium alloys used as cladding material in nuclear power reactors. C-ring samples, machined from cladding tubes in a recrystallised and cold worked condition, were subjected to compressive stress while submerged in an iodine-ethanol solution to simulate stress corrosion cracks arising from pellet cladding interaction. The complex morphology of these stress corrosion cracks was imaged in 3D using X-ray computed tomography (XCT), and subsequent analysis using both 2D and 3D electron backscatter diffraction (EBSD) allowed for the interaction of these cracks with microstructure to be investigated. Intergranular cracking modes were observed to dominate in the recrystallised microstructure, resulting in cracking in the radial direction with variations on the order of the grain size. Crack propagation in the cold worked microstructure was observed to be correlated with the direction of the elongated grains, resulting in a more tangential crack path with less local variation and a microstructure potentially more susceptible to iodine-induced stress corrosion cracking. 3D-EBSD using serial sectioning allows for the determination of the full five-parameter grain boundary description, and opens up the possibility of a statistical analysis of susceptible boundaries to SCC. Nanoscale secondary ion mass spectrometry (NanoSIMS) was also used to map the chemical distribution in the crack tip region and provides possible evidence of iodine segregation ahead of the crack tip. The results provide new insight into crack propagation mechanisms in recrystallised and cold worked microstructures, and pave the way for a more mechanistic understanding of crack propagation through advanced characterisation of iodine-induced stress corrosion cracks in zirconium alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Austenite and precipitation in secondary-hardening ultra-high-strength stainless steel

Highlights: • Austenite and precipitation in Ferrium S53 steel were analyzed. • Austenite decreased to less than 5% after cryogenic treatment and tempering. • M{sub 2}C carbide could segregate inside martensite lath or in the larger parallel microstructure. - Abstract: Ferrium S53 is a new secondary-hardening ultra-high-strength stainless steel, with more Cr than other Co-Ni ultra-high-strength steels. Austenite has a great effect on the fracture toughness of this metal, and the carbides that are precipitated are the main strengthening phase of Ferrium S53 steel; in this study, its microstructural changes during heat treatment were observed and analyzed by X-ray diffraction (XRD), Optical microscope (OM), SEM, and transmission electron microscopy (TEM). About 40.85% retained austenite in the quenched sample is decreased to less than 5% after cryogenic treatment and tempering. In the final sample, block austenite is retained austenite, and film austenite around 5 nm in width is reverted austenite. Inside the martensite lath, parallel twin-like structures are actually segregated M{sub 2}C precipitates, and most of them are smaller than 20 nm. These precipitates can be aggregated into a several-micron-long parallel zonal microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Controlling homogenization length scales and microstructure in additively manufactured Ti-Ta functionally graded materials

Materials with smooth compositional gradients or functionally grade materials (FGMs) produced via additive manufacturing (AM), enables joining dissimilar materials and optimizing multiple properties in advanced engineering applications. However, as-printed AM microstructures exhibit micro-segregation and solidification defects which, when combined with controlling macroscale gradient properties, complicates necessary post-processing. Here, we use CALPHAD-informed diffusion modelling to design post-processing heat treatments for lightweight to refractory FGMs. Ti-Ta (0 to 85 at. % Ta) FGMs were fabricated using laser-based directed energy deposition AM. Post-processing heat treatments at 1000° C and 1500° C were designed to promote homogenization across specific length scales and experimentally validated. Investigation of chemical segregation and microstructures demonstrated that the length scale of homogenization is controlled as a function of time, temperature, and local composition. Ta-rich regions exhibited incomplete homogenization compared to Ti-rich layers. Unmelted Ta particles were found to completely dissolve at 1500 °C. By controlling cooling rate (200 °C/min), martensitic structures were produced between 14–36 at. % Ta, consistent with martensite-start temperatures calculations, while furnace cooling (2 °C/min) produced α+β morphologies. This work establishes a validated predictive framework for designing post-processing to tailor microstructure and chemical architecture in AM FGMs, facilitating their deployment in demanding environments.

Materials science↗
DOE OSTI2012

Room temperature ferromagnetism in Co doped ZnO within an optimal doping level of 5%

Highlights: ► Zn{sub 1−x}Co{sub x}O ((0 ≤ x ≤ 0.1)) system synthesized by solid state reaction technique. ► Observation of room temperature ferromagnetism for 3 and 5% Co doped ZnO. ► XPS and EPMA studies predict the occurrence of segregated CoO clusters. ► Suppresses ferromagnetic ordering in higher doping percentage of Co (>5%). -- Abstract: We report on the structural, micro-structural and magnetic properties of Zn{sub 1−x}Co{sub x}O (0 ≤ x ≤ 0.1) system. Electron probe micro-structural analysis on 5% Co doped ZnO indicates the presence of segregated cobalt oxide which is also confirmed from the Co 2p core level X-ray photoelectron spectrum. The presence of oxygen defects in lower percentage of Co doped ZnO (≤5%) enhances the carrier mediated exchange interaction and thereby enhancing the room-temperature ferromagnetic behaviour. Higher doping percentage of cobalt (>5%) creates weak link between the grains and suppresses the carrier mediated exchange interaction. This is the reason why room temperature ferromagnetism is not observed in 7% and 10% Co doped ZnO.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Nanostructured columnar heterostructures of TiO{sub 2} and Cu{sub 2}O enabled by a thin-film self-assembly approach: Potential for photovoltaics

Graphical abstract: Display Omitted Highlights: ► Material self-assembly in phase-separated oxides is exploited. ► Three-dimensionally nanostructured epitaxial films are grown using sputtering. ► Films are composed of well-ordered oriented nanopillars of n-type TiO{sub 2} and p-type Cu{sub 2}O. ► Observed interfaces at adjacent TiO{sub 2}–Cu{sub 2}O columns are nearly atomically distinct. ► Absorption profile of the composite film captures a wide range of the solar spectrum. -- Abstract: Significant efforts are being devoted to the development of multifunctional thin-film heterostructures and nanostructured material architectures for components with novel applications of superconductivity, multiferroicity, solar photocatalysis and energy conversion. In particular, nanostructured assemblies with well-defined geometrical shapes have emerged as possible high efficiency and economically viable alternatives to planar photovoltaic thin-film architectures. By exploiting phase-separated self-assembly, here we present advances in a vertically oriented two-component system that offers potential for future development of nanostructured thin film solar cells. Through a single-step deposition by magnetron sputtering, we demonstrate growth of an epitaxial, composite film matrix formed as self-assembled, well ordered, phase segregated, and oriented nanopillars of n-type TiO{sub 2} and p-type Cu{sub 2}O. The composite films were structurally characterized to atomic resolution by a variety of analytical tools, and evaluated for preliminary optical properties using absorption measurements. We find nearly atomically distinct TiO{sub 2}–Cu{sub 2}O interfaces (i.e., needed for possible active p–n junctions), and an absorption profile that captures a wide range of the solar spectrum extending from ultraviolet to visible wavelengths. This high-quality materials system could lead to photovoltaic devices that can be optimized for both incident light absorption and carrier collection.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

Formation of large loop-hydrogen complexes and related effects on mechanical properties of Zirconium investigated with molecular dynamics method

Here, using molecular dynamics (MD) method, interaction between hydrogen (H) atoms and interstitial or vacancy dislocation loops in Zr is extensively studied. The results show that the binding of hydrogen atoms to dislocation loops is anisotropic (attractive or repulsive), depending on the position of the hydrogen atoms with respect to the loop’s core. The anisotropy is governed by excess volume and stress field induced by the loop. For a 1/3[$2\bar1$$\bar1$$0$] interstitial dislocation loop, hydrogen atoms preferentially segregate near the outside of the loop and close to the decomposition knots of the loop. While for a 1/3[$2\bar1$$\bar1$$0$] or 1/6[$20$$\bar2$$3$] vacancy loop, hydrogen atoms prefer to segregate near the inside of the loop. The present work indicates large loop-hydrogen complexes could form in Zr. The binding of hydrogen to loops is stable up to 600 K, while dissociation is observed at 900 K. Formation of loop-hydrogen complexes affect the activation of slip system, resulting in higher yield stress of Zr. The effect increases with the increasing ratio of H to vacancies or interstitials in the vacancy or interstitial loops. The results imply the effects of large loop-hydrogen complexes should be considered to fully understand radiation damage in Zr.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Partitioning of tramp elements Cu and Si in a Ni-based superalloy and their effect on creep properties

An alloy's processing history, including melting, remelting or the choice of stock material, affects its purity and eventually involves tramp element pickup or retention. Herein, variants of a novel Ni-based superalloy were manufactured with different levels of purity. The so-called low purity alloys contained 0.138 wt. % Cu and 0.019 wt. % Si while the Cu and Si levels were below x-ray fluorescence (XRF) detection limits of 0.003 and 0.010 wt. %, respectively, in the high purity ingots. Atom-probe tomography (APT) was carried out and revealed Si partitioning at the following interfaces: grain boundaries, MC carbide/γ, M 3 B 2 boride/$γ$ and M 3 B 2 boride/$γ$'. Copper was found to primarily segregate to the $γ$' precipitates. An average of 2.4 × decrease in creep life and 4.3 × decrease in creep ductility was measured in the low purity alloys, which was attributed to the embrittlement caused by Si segregation to grain boundaries. Furthermore, the positive effect of B on the creep properties was mitigated by the presence of Si. Thermodynamic predictions for the matrix and γ' precipitate compositions represented the trends observed experimentally although the extent of preferential partitioning lacks accuracy. Monte Carlo simulations were performed to describe the partitioning of Cu and Si atoms to either $γ$ or $γ$' phases.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Irradiation-induced formation of G-phase precipitates and M 2 X carbides in self-ion irradiated HT-9

Ferritic-martensitic steels with high chromium content are a promising material group for advanced nuclear systems due to their high temperature strength and good irradiation tolerance. HT-9 is an optimized and often-studied alloy in this group, but additional studies are required on its radiation response under extreme conditions to be experienced in various types of nuclear reactors, especially with respect to phase stability under irradiation. Self-ion irradiation of HT-9 by 5 MeV Fe ions was used to simulate neutron-induced behavior reaching peak doses of 100 and 300 dpa at temperatures ranging from 450 to 550 °C. M 23 C 6 carbides that existed prior to irradiation were found to remain stable under all examined irradiation conditions. As irradiation progressed at 450 and 500 °C, however, formation of spherical-like G-phase precipitates and needle-like M 2 X carbides was observed. G-phase precipitates were found to be enriched in Ni, Si, and Mn, and show no interface segregation, whereas needle-like M 2 X carbides were rich in Cr and Mo and clearly displayed interface segregation of Ni and Si. M 2 X carbide formation is believed to be assisted by vacancies, while G-phase precipitation is thought to be assisted by interstitials. Finally, this difference in defect-mediated formation leads to a difference in distribution with depth. M 2 X carbides are distributed over shallower depths than that of G-phase precipitates, consistent with defect imbalance predictions that consider the influence of the injected interstitial effect.

atom probe tomography↗
DOE OSTI2022

($\mathrm{INVITED}$)Counter-ion effect on the diffusion behavior of $\mathrm{Y}$b, $\mathrm{L}$u, and $\mathrm{N}$d ions in $\mathrm{YAG}$ transparent ceramics

The ability to fabricate additively manufactured laser waveguides with sharp dopant concentration interfaces is limited by diffusion of the dopants at the temperatures required to fully densify the material. Compositional analysis of bilayer samples, where each layer was either undoped YAG or YAG doped with Yb, Lu, or Nd, were fabricated such that all combinations were available for testing. Samples were fabricated at both 1750°C and 1850°C to determine the diffusion behavior of each dopant alone and also in the presence of a second dopant. It was found that the experimental concentration profiles exhibited both intragranular (bulk) and grain boundary contributions, and thus fitting to a complementary error function equation required the use of two diffusion coefficients. Nd always diffused further along grain boundaries than the other dopants, due in part to its small segregation coefficient in YAG. It is shown that the presence of Nd as a counter dopant inhibits intragranular diffusion of other dopants while enhancing their grain boundary diffusion. All the observed trends were attributed to a combination of intragranular lattice strain due to: dopant ions replacing yttrium substitutionally, the relative driving forces for the segregation of dopant ions to grain boundaries, and the ability of one dopant to affect the diffusion of a different dopant in the other direction to maintain charge neutrality.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Characteristics of the sub-micron ash aerosol generated during oxy-coal combustion at atmospheric and elevated pressures

This paper is concerned with the effect of pressure on the particle size distribution and the size-segregated composition of the sub-micron ash aerosol created during oxy-coal combustion under near practical self-sustaining combustion conditions. The problem is important because pressurized oxy-coal combustion has been proposed as one promising technology to minimize CO 2 emissions. Sub-micron ash plays a major role in ash deposition mechanisms, which, in turn, can control boiler performance. In this work, the same bituminous coal was burned at pressures of 1, 8 and 15 bar in O 2 /CO 2 environments. Here, tests employed a 100 kW (rated) oxy-fuel combustor (OFC) operated at atmospheric pressure (1 bar) and a 300 kW (rated) entrained-flow pressurized reactor (EFPR) at elevated pressures (8 and 15 bar). Although these tests were conducted under near practical combustion conditions, confounding effects of peak flame temperature variations were minimized for the 1 bar and 15 bar tests, allowing the role of elevated pressure to be isolated. For the EFPR tests, a specially designed sampling system was used to sample sub-micron ash aerosols from the pressurized combustor and is described in detail. Results showed that at the same peak temperature but higher pressure, the fractions of ash aerosol partitioned into the PM 0.6 and PM 1 size fractions were greatly diminished. Moreover, elevated pressures caused significant changes in the composition of the (size-segregated) sub-micron aerosol, especially in its alkali content, which increased significantly. Examination of fractions of each element that ended up in the sub-micron fume suggested that, at constant temperature, the effect of pressure on vaporization of semi-volatile metals was very different from that on the release into the gas phase of non-volatile metals and could not be explained by equilibrium.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Aerosol detection efficiency in inductively coupled plasma mass spectrometry

We used an electrostatic size classification technique to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Moreover, we counted size-segregated particles with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10 -5 to 10 -11 . Free molecular heat and mass transfer theory was applied, but evaporative phenomena were not sufficient to explain the dependence of aerosol detection on particle diameter. Additional work is needed to correlate experimental data with theory for metal-oxides where thermodynamic property data are sparse relative to pure elements. Finally, when matrix effects and the diffusion of ions inside the plasma were considered, mass loading was concluded to have had an effect on the dependence of detection efficiency on particle diameter.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗