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All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Facet-Specific Stability of ZIF-8 in the Presence of Acid Gases Dissolved in Aqueous Solutions

ZIF-8 is a crystalline microporous material that has been widely studied because of its thermal and chemical stability relative to other metal–organic frameworks (MOFs) and its potential for use in a number of gas adsorption, separation, and catalysis applications. However, most studies focus on characterization of the bulk structure of ZIF-8, ignoring the potential effect of the particle shape and the external surface on these applications. This report describes studies that examined the stability of the {110} and {100} crystallographic facets of ZIF-8 under mildly acidic conditions. Though the {110} facet is more thermodynamically stable than the {100} facet, it is found to be more susceptible to degradation by acid exposure. It is hypothesized that the mechanism of particle degradation follows a shrinking-core model, with surface imidazolates being replaced by hydroxyls, as suggested by complementary X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy characterization. Computational investigations support this hypothesis and suggest that the reaction energy for insertion of water into the Zn–MeIm bond is more favorable on the {110} facet than on the {100} facet because of steric constraints. Additionally, the reaction energies are more favorable on both surfaces in the presence of SO 2 . These findings have implications for the formation of surface barriers that can affect mass transfer into or out of the ZIF crystals. This study represents the first comprehensive investigation of differences between exposed surface facets of a MOF.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Fluorescence-Correlation Spectroscopy Study of Molecular Transport within Reversed-Phase Chromatographic Particles Compared to Planar Model Surfaces

Reversed-phase liquid chromatography (RPLC) is a widely used technique for molecular separations. Stationary-phase materials for RPLC generally consist of porous silica-gel particles functionalized with n-alkane ligands. Understanding motions of molecules within the interior of these particles is important for developing efficient chromatographic materials and separations. To characterize these dynamics, time-resolved spectroscopic methods (photobleach recovery, fluorescence correlation, single-molecule imaging) have been adapted to measure molecular diffusion rates, typically at n-alkane-modified planar silica surfaces, which serve as models of chromatographic interfaces. A question arising from these studies is how dynamics of molecules on a planar surface relate to motions of molecules within the interior of a porous chromatographic particle. In this paper, imaging-fluorescence-correlation spectroscopy is used to measure diffusion rates of a fluorescent probe molecule 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbocyanine perchlorate (DiI) within authentic RPLC porous silica particles and compared with its diffusion at a planar C18-modified surface. The results show that surface diffusion on the planar C18 substrate is much faster than the diffusion rate of the probe molecule through a chromatographic particle. Surface diffusion within porous particles, however, is governed by molecular trajectories along the tortuous contours of the interior surface of the particles. By accounting for the greater surface area that a molecule must explore to diffuse macroscopic distances through the particle, the molecular-scale diffusion rates on the two surfaces can be compared, and they are virtually identical. Furthermore, these results provide support for the relevance of surface-diffusion measurements made on planar model surfaces to the dynamic behavior of molecules on the internal surfaces of porous chromatographic particles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Impact of Materials Processing on Microstructural Evolution and Hydrogen Isotope Storage Properties of Pd-Rh Alloy Powders.

Cryomilled Pd - 10Rh was investiga ted as potential solid - state storage material of hydrogen. Pd - 10Rh was first atomized, and then subsequently cryomilled. The cryomilled Pd - 10Rh was then examined using microstructural characterization techniques including op tical microscopy, electron microscopy, and X - ray diffraction. Pd - 10Rh particles were significantly flattened, increasing the apparent surface area. Microstructural refinement was observed in the cryomilled Pd - 10Rh, generating grains at the nanom etric scale through dislocation - based activity. Hydrogen sorption properties were also characterized, generating both capacity as well as kinetics measurements. It was found that the microstructural refinement due to cryomilling did not play a significant role on hyd rogen sorption properties until the smallest grain size (on the order of %7E25 nm) was achieved. Additionally, the increased surface area and other changes in particle morphology were associated with cryomilling changed the kinetics of hydrogen absorption.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The stress, surface spin and dipolar interaction in the diluted NiFe{sub 2}O{sub 4} nanoparticles by the SiO{sub 2} matrix: Characterization and analyses

Well-dispersed uniform NiFe{sub 2}O{sub 4} nanoparticles (NPs) with an average particle size of 15.4 nm were synthesized by thermal decomposition of a metal–organic salt, and then were diluted in a SiO{sub 2} matrix via a sol–gel method with different concentration. The magnetization (M) dependence of NiFe{sub 2}O{sub 4}/SiO{sub 2} on the temperature (T) and on the applied magnetic field (H) was systematically characterized by the Quantum Design superconducting quantum interference device (SQUID) PPMS system. The results of M ~ H/T divide the magnetic properties between 10 K and 300 K into two regions: the low temperature blocked-particle regime below the blocking temperature T{sub B} and the interacting superparamagnetic (ISP) regime above T{sub B}. In the ISP regime, all samples deviate from the ideal Langevin superparamagnetic behavior due to the effective anisotropy induced by the stress, surface spins and interparticle dipolar interaction. The Raman spectra indicate that the stress in all samples exhibits the vibration behavior, which leads to the effective anisotropy and hence coercivity vibration. - Graphical abstract: Display Omitted - Highlights: • Increase of NiFe{sub 2}O{sub 4} NPs' concentration elevates T{sub B} and broadens ZFC peak. • NiFe{sub 2}O{sub 4}/SiO{sub 2} samples do not exhibit the ideal superparamagnetism above T{sub B}. • Stress leads to the effective anisotropy and hence H{sub c} vibration. • Stress vibration was characterized in detail by the Raman spectra.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Schottky Noise and Beam Transfer Functions

Beam transfer functions (BTF)s encapsulate the stability properties of charged particle beams. In general one excites the beam with a sinusoidal signal and measures the amplitude and phase of the beam response. Most systems are very nearly linear and one can use various Fourier techniques to reduce the number of measurements and/or simulations needed to fully characterize the response. Schottky noise is associated with the finite number of particles in the beam. This signal is always present. Since the Schottky current drives wakefields, the measured Schottky signal is influenced by parasitic impedances.

43 PARTICLE ACCELERATORS↗
DOE OSTI2016

Green Ocean Amazon (GoAmazon) 2014/15. Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SVTAG) Field Campaign Report

In areas where biogenic emissions are oxidized in the presence of anthropogenic pollutants such as SO2, NOx, and black carbon, it has become increasingly apparent that secondary organic aerosol (SOA) formation from biogenic volatile organic compounds (VOCs) is substantially enhanced. Research is urgently needed to elucidate fundamental processes of natural and anthropogenically influenced VOC oxidation and the contribution of these processes to SOA formation. GoAmazon 2014/15 afforded study of the chemical transformations in the region downwind of Manaus, Brazil, where local biogenic VOC emissions are high, and their chemical oxidation can be studied both inside and outside of the urban plume to differentiate the role of anthropogenic influence on secondary aerosol formation during oxidation of these natural VOC emissions. To understand the connection between primary biogenic VOC emissions and their secondary products that form aerosols, we made time-resolved molecular level measurements by deploying a Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SV-TAG) and a sequential filter sampler during two intensive operational periods (IOPs) of the GoAmazon 2014/15 field campaign. The SV-TAG measured semi-volatile organic compounds in both the gas and particle phases and the sequential filter sampler collected aerosols on quartz fiber filters in four-hour increments used for offline analysis. SV-TAG employed novel online derivatization that provided chemical speciation of highly oxygenated or functionalized compounds that comprise a substantial fraction of secondary organic aerosols, yet are poorly characterized. It also provided partitioning of these compounds between the vapor and particle phases at sufficient time resolution to define the importance of competing atmospheric processes. These measurements were supported by offline analysis of the filters using two-dimensional gas chromatography (GC x GC) with high-resolution time-of-flight mass spectrometry (HR-TOF-MS) using both electron impact (EI) and soft vacuum ultraviolet (VUV) ionization with derivatization. Speciated chemical data from SV-TAG and filter measurements were used to elucidate the relative importance of potential oxidation pathways by providing detailed information on the product distribution from atmospheric reactions and the quantification of known tracers for various oxidation pathways. Together, these techniques provided unequivocal molecular identification of a wide range of atmospheric organic compounds spanning the volatile, semi-volatile, and non-volatile phases. This level of chemical characterization provided insight into the chemical and physical processes that control the atmospheric oxidation of biogenic VOC and subsequent formation of SOA.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Direct observation of ice nucleation events on individual atmospheric particles

Heterogeneous ice nucleation is a physical chemistry process of critical relevance to a range of topics in the fundamental and applied sciences and technologies. Heterogeneous ice nucleation remains insufficiently understood, partially due to the lack of experimental methods capable of obtaining in situ microscopic details of ice formation over nucleating substrates or particles. Here, we present microscopic observations of ice nucleation events on kaolinite particles at the nanoscale and demonstrate the capability of direct tracking and micro-spectroscopic characterization of individual ice nucleating particles (INPs) in an authentic atmospheric sample. Furthermore, this approach utilizes a custom-built ice nucleation cell, interfaced with an Environmental Scanning Electron Microscope (IN-ESEM platform) operated at temperatures and relative humidities relevant for heterogeneous ice nucleation. The IN-ESEM platform allows dynamic observations of individual ice formation events over particles in isobaric and isothermal experiments. Isothermal experiments on individual kaolinite particles demonstrate that ice crystals preferably nucleate at the edges of the stacked kaolinite platelets, rather than on their basal planes. Finally, these experimental observations of the location of ice nucleation provide direct information for further theoretical chemistry predictions of ice formation on kaolinite.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2003

Water Atomization of Barium Fluoride: Calcium Fluoride for Enhanced Flow Characteristics of PS304 Feedstock Powder Blend

PS304 is a plasma spray deposited solid lubricant coating with feedstock composed of NiCr, Cr2O3, Ag, and BaF2-CaF2 powders. The effects of rounded BaF2-CaF2 particles on the gravity-fed flow characteristics of PS304 feedstock have been investigated. The BaF2-CaF2 powder was fabricated by water atomization using four sets of process parameters. Each of these powders was then characterized by microscopy and classified by screening to obtain 45 to 106 micron particles and added incrementally from 0 to 10 wt% to the other constituents of the PS304 feedstock, namely nichrome, chromia, and silver powders. The relationship between feedstock flow rate, measured with the Hall flowmeter, and concentration of fluorides was found to be linear in each case. The slopes of the lines were between those of the linear relationships previously reported using angular and spherical fluorides and were closer to the relationship predicted using the rule of mixtures. The results offer a fluoride fabrication technique potentially more cost-effective than gas atomization processes or traditional comminution processes.

Stanford, Malcolm K.↗
DOE OSTI2016

Characterization of electrical properties in axial Si-Ge nanowire heterojunctions using off-axis electron holography and atom-probe tomography

Doped Si-Ge nanowire (NW) heterojunctions were grown using the vapor-liquid-solid method with AuGa and Au catalyst particles. Transmission electron microscopy and off-axis electron holography (EH) were used to characterize the nanostructure and to measure the electrostatic potential profile across the junction resulting from electrically active dopants, while atom-probe tomography (APT) was used to determine the Si, Ge and total (active and inactive) dopant concentration profiles. A comparison of the measured potential profile with simulations indicated that Ga dopants unintentionally introduced during AuGa catalyst growth were electronically inactive despite APT results that showed considerable amounts of Ga in the Si region. 10% P in Ge and 100% B in Si were estimated to be activated, which was corroborated by in situ electron-holography biasing experiments. This combination of EH, APT, in situ biasing and simulations allows a better knowledge and understanding of the electrically active dopant distributions in NWs.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Gauge-invariant perturbation expansion in powers of electric charge for the density-of-states of a network model for charged-particle motion in a uniform background magnetic flux density

An explicitly gauge-invariant expansion in powers of e/$\hbar$ times the magnetic flux density is formally obtained for the density of states [as characterized by the trace of the resolvent $\hat{G}$ = (ω-$\hat{ℎ}$)-1] of a charged particle moving on a Hermitian quantum network that is embedded in a Euclidean background that supports a uniform magnetic flux density. The explicit expressions, given here up to third order in the flux density, are also valid for the “local trace” (the trace of $\hat{P}_i\hat{G}$ , where $\hat{P}_i$ is the projector on a network node) and do not appear to have been previously given.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

The effect of BaTiO{sub 3} particle shape on complex permittivity of 0.98MgTiO{sub 3}–0.02BaTiO{sub 3} composite powders at GHz frequencies

Highlights: • Elongated micrometre sized BaTiO{sub 3} particles had strong effect on permittivity. • Effect was significantly stronger compared to μm and nm sized spherical particles. • Properties could be tailored by varying the particle shapes of dielectric powders. • Could be utilized, e.g., in a production of electrical composites for RF applications. - Abstract: The effect of BaTiO{sub 3} particle shape on the properties of 0.98MgTiO{sub 3}–0.02BaTiO{sub 3} composite powders was characterized and analyzed using an indirectly coupled open-ended coaxial cavity resonator at gigahertz frequencies. Elongated micrometre sized BaTiO{sub 3} particles were found to have a significantly stronger effect on permittivity when compared to composite powders having micro and nano sized spherical BaTiO{sub 3} particles. Inclusion permittivities and dielectric loss tangents of composite powders increased from that of pure MgTiO{sub 3} powder, 13.3 and 4.6 × 10{sup −3}, up to 15.7 and 1.7 × 10{sup −2} with needle shaped BaTiO{sub 3} particles, respectively. The presented results give valuable information for tailoring the properties of dielectrics which can be utilized in the vast field of electronic component manufacturing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Regularized inversion of aerosol hygroscopic growth factor probability density function: application to humidity-controlled fast integrated mobility spectrometer measurements

Abstract. Aerosol hygroscopic growth plays an important role in atmospheric particle chemistry and the effects of aerosol on radiation and hence climate. The hygroscopic growth is often characterized by a growth factor probability density function (GF-PDF), where the growth factor is defined as the ratio of the particle size at a specified relative humidity to its dry size. Parametric, least-squares methods are the most widely used algorithms for inverting the GF-PDF from measurements of the humidified tandem differential mobility analyzer (HTDMA) and have been recently applied to the GF-PDF inversion from measurements of the humidity-controlled fast integrated mobility spectrometer (HFIMS). However, these least-squares methods suffer from noise amplification due to the lack of regularization in solving the ill-posed problem, resulting in significant fluctuations in the retrieved GF-PDF and even occasional failures of convergence. In this study, we introduce nonparametric, regularized methods to invert the aerosol GF-PDF and apply them to HFIMS measurements. Based on the HFIMS kernel function, the forward convolution is transformed into a matrix-based form, which facilitates the application of the nonparametric inversion methods with regularizations, including Tikhonov regularization and Twomey's iterative regularization. Inversions of the GF-PDF using the nonparameteric methods with regularization are demonstrated using HFIMS measurements simulated from representative GF-PDFs of ambient aerosols. The characteristics of reconstructed GF-PDFs resulting from different inversion methods, including previously developed least-squares methods, are quantitatively compared. The result shows that Twomey's method generally outperforms other inversion methods. The capabilities of Twomey's method in reconstructing the pre-defined GF-PDFs and recovering the mode parameters are validated.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

Characterization of a detector chain using a FPGA-based time-to-digital converter to reconstruct the three-dimensional coordinates of single particles at high flux

We report on the development of a novel FPGA-based time-to-digital converter and its implementation in a detection chain that records the coordinates of single particles along three dimensions. The detector is composed of micro-channel plates mounted on top of a cross delay line and connected to fast electronics. We demonstrate continuous recording of the timing signals from the cross delay line at rates up to 4.1 × 10{sup 6} s{sup −1} and three-dimensional reconstruction of the coordinates up to 3.2 × 10{sup 6} particles per second. From the imaging of a calibrated structure we measure the in-plane resolution of the detector to be 140(20) μm at a flux of 3 × 10{sup 5} particles per second. In addition, we analyze a method to estimate the resolution without placing any structure under vacuum, a significant practical improvement. While we use UV photons here, the results of this work apply to the detection of other kinds of particles.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2017

Multifield stochastic particle production: beyond a maximum entropy ansatz

In this work, we explore non-adiabatic particle production for N f coupled scalar fields in a time-dependent background with stochastically varying effective masses, cross-couplings and intervals between interactions. Under the assumption of weak scattering per interaction, we provide a framework for calculating the typical particle production rates after a large number of interactions. After setting up the framework, for analytic tractability, we consider interactions (effective masses and cross couplings) characterized by series of Dirac-delta functions in time with amplitudes and locations drawn from different distributions. Without assuming that the fields are statistically equivalent, we present closed form results (up to quadratures) for the asymptotic particle production rates for the N f =1 and N f =2 cases. We also present results for the general N f >2 case, but with more restrictive assumptions. We find agreement between our analytic results and direct numerical calculations of the total occupation number of the produced particles, with departures that can be explained in terms of violation of our assumptions. We elucidate the precise connection between the maximum entropy ansatz (MEA) used in Amin & Baumann (2015) and the underlying statistical distribution of the self and cross couplings. We provide and justify a simple to use (MEA-inspired) expression for the particle production rate, which agrees with our more detailed treatment when the parameters characterizing the effective mass and cross-couplings between fields are all comparable to each other. However, deviations are seen when some parameters differ significantly from others. We show that such deviations become negligible for a broad range of parameters when N f >> 1.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2019

The effect of thermal-aging on the microstructure and mechanical properties of 9Cr ferritic/martensitic ODS alloy

In this paper, the thermal-stability of 9Cr F/M ODS alloy was evaluated by the aging treatment in the air at 700 degrees C for 10 h, 100 h, 1000 h, and 2005 h. The variations of mechanical properties with different aging periods were tested in terms of tensile testing and vickers microhardness. And the microstructural evolution of strengthening particles and grain morphologies in the 9Cr F/M ODS alloys were characterized using field emission scanning electron microscopy, transmission electron microscopy and high-energy X-ray diffraction. It was found that the as-rolled 9Cr F/M ODS alloy slightly recovered without recrystallization during the initial stage of less than 10 h aging time, resulting in the slight loss of tensile strength and microhardness and the increase of elongation. With the aging time prolonged to 2005 h, several of nano-sized Y-Ti-O particles coarsened and the composition changed to Y-Ti-Al-O, and the number density of large size nitride precipitations increased and the composition also changed from TiN to (Ti,AI)N. Meanwhile, some of grains tend to grow up in some preferential directions due to the zener pinning effect by the localized uneven distributed particles inside the grains, causing more particles, especially the particles with a size of larger than 40 nm, located at grain boundaries. These microstructural evolutions lead to the increasing of microhardness and a little bit decreasing of eleongation during 10 h-2005 h, and the increasing of tensile strength during 10 h-1000 h with the subsequent slight decreasing during 1000 h-2005 h. In conclusion, 9Cr F/M alloy shows a relatively good thermal-aging stability at 700 degrees C for 2005 h.

36 MATERIALS SCIENCE↗
DOE OSTI2017

A novel partitioning method for block-structured adaptive meshes

We propose a novel partitioning method for block-structured adaptive meshes utilizing the meshless Lagrangian particle concept. With the observation that an optimum partitioning has high analogy to the relaxation of a multi-phase fluid to steady state, physically motivated model equations are developed to characterize the background mesh topology and are solved by multi-phase smoothed-particle hydrodynamics. In contrast to well established partitioning approaches, all optimization objectives are implicitly incorporated and achieved during the particle relaxation to stationary state. Distinct partitioning sub-domains are represented by colored particles and separated by a sharp interface with a surface tension model. In order to obtain the particle relaxation, special viscous and skin friction models, coupled with a tailored time integration algorithm are proposed. Numerical experiments show that the present method has several important properties: generation of approximately equal-sized partitions without dependence on the mesh-element type, optimized interface communication between distinct partitioning sub-domains, continuous domain decomposition which is physically localized and implicitly incremental. Therefore it is particularly suitable for load-balancing of high-performance CFD simulations.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2019

Laboratory and field evaluation of the Aerosol Dynamics Inc. concentrator (ADIc) for aerosol mass spectrometry

Abstract. An air-to-air ultrafine particle concentrator (Aerosol Dynamics Inc. concentrator; ADIc) has been designed to enhance online chemical characterization of ambient aerosols using aerosol mass spectrometry. The ADIc employs a three-stage, moderated water-based condensation growth tube coupled to an aerodynamic focusing nozzle to concentrate fine particles into a portion of the flow. The system can be configured to sample between 1.0 and 1.7 L min -1 , with an output concentrated flow between 0.08 and 0.12 L min -1 , resulting in a theoretical concentration factor (sample flow/output flow) ranging from 8 to 21. Laboratory tests with monodisperse particles show that the ADIc is effective for particles as small as 10 nm. Laboratory experiments conducted with the Aerosol Mass Spectrometer (AMS) showed no shift in the particle size with the ADIc, as measured by the AMS particle time-of-flight operation. The ADIc-AMS system was operated unattended over a 1-month period near Boston, Massachusetts. Comparison to a parallel AMS without the concentrator showed concentration factors of 9.7±0.15 and 9.1±0.1 for sulfate and nitrate, respectively, when operated with a theoretical concentration factor of 10.5±0.3. The concentration factor of organics was lower, possibly due to the presence of large particles from nearby road-paving operations and a difference in aerodynamic lens cutoff between the two AMS instruments. Another field deployment was carried out in Helsinki, Finland. Two ~10 d measurement periods showed good correlation for the concentrations of organics, sulfate, nitrate and ammonium measured with an Aerosol Chemical Speciation Monitor (ACSM) with the ADIc and a parallel AMS without the concentrator. Additional experiments with an AMS alternating between the ADIc and a bypass line demonstrated that the concentrator did not significantly change the size distribution or the chemistry of the ambient aerosol particles.

47 OTHER INSTRUMENTATION↗
NASA NTRS1993

Preliminary AEM study of the microstructure and composition of metal particles in ordinary chondrites

The purpose of this study is to examine the microstructure and composition of the metal particles in ordinary chondrites using analytical electron microscopy (AEM) techniques. Since the phases produced within the metal particles are very fine, the application of various AEM techniques for structural and chemical characterization is critical. However, thin specimen preparation for AEM study has proven very difficult because of the matrix silicate which is present. This is the first AEM study of the metal particles in chondrites. A type 6 chondrite, Saint Severin (LL6), was selected for examination because the metal phases have been reheated into the single phase taenite region (greater than 700 C), and cooled slowly to lower temperatures. A combination of electron optical instruments was employed including a field emission gun (FEG) JEOL 840F high resolution scanning electron microscope (HRSEM), a JEOL 6300F FEG-HRSEM, a Philips 400T AEM, and a JEOL 733 electron probe microanalyzer (EPMA).

Yang, C. W.↗