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DOE OSTI2024

Techno-economic and life-cycle analysis of strategies for improving operability and biomass quality in catalytic fast pyrolysis of forest residues

Many of the challenges faced by the first commercial biorefineries were associated with feedstock handling, quality, and cost. Strategies are needed to enable further expansion of biorefineries and meet the growing demand for bio-based fuels and products. Here, we examine 2 key feedstock challenges and mitigation strategies in the context of a catalytic fast pyrolysis (CFP) biorefinery: (1) the operability of the feed system, which may be improved by modifying the minimum particle size fed to the reactor, and (2) the quality of the biomass, which may be improved by employing air classification to remove undesirable material and increase fuel yields. We conduct techno-economic analysis (TEA) and life-cycle analysis for these strategies, employing a discrete event simulation model for biomass preprocessing combined with a series of correlations developed from literature data and a rigorous CFP conversion model. Our results highlight the importance of balancing increased cost and material losses from preprocessing against improved operability and fuel yields. Economics and sustainability were optimized when operating at the lowest minimum particle size, emphasizing the importance of minimizing material losses while maintaining the operability of the process. Economically, additional costs and material losses from air classification could be acceptable due to improved biomass conversion, and an optimum air classification speed was identified; however, the fuel GHG emissions were minimized when air classification was not used. Valorizing material removed during preprocessing as a coproduct could improve economics and sustainability, decreasing the burden of material losses.

09 - BIOMASS FUELS↗

DOE OSTI2019

Single‐Particle Tracking for Understanding Polydisperse Nanoparticle Dispersions

Abstract Colloidal dispersions of nanomaterials are often polydisperse in size, significantly complicating their characterization. This is particularly true for materials early in their historical development due to synthetic control, dispersion efficiency, and instability during storage. Because a wide range of system properties and technological applications depend on particle dimensions, it remains an important problem in nanotechnology to identify a method for the routine characterization of polydispersity in nanoparticle samples, especially changes over time. Commonly employed methods such as dynamic light scattering or analytical ultracentrifugation (AUC) accurately estimate only the first moment of the distribution or are not routine. In this work, the use of single‐particle tracking (SPT) to probe size distributions of common nanoparticle dispersions, including polystyrene nanoparticles, single‐walled carbon nanotubes, graphene oxide, chitosan‐tripolyphosphate, acrylate, hexagonal boron nitride, and poly(lactic‐ co ‐glycolic acid), is proposed and explored. The analysis of particle tracks is conducted using a newly developed Bayesian algorithm that is called Maximum A posteriori Nanoparticle Tracking Analysis. By combining SPT and AUC techniques, it is shown that it is possible to independently estimate the mean aspect ratio of anisotropic particles, an important characterization property. It is concluded that SPT provides a facile, rapid analytical method for routine nanomaterials characterization.

Gong, Xun↗

DOE OSTI2015

Quantitative study of particle size distribution in an in-situ grown Al–TiB{sub 2} composite by synchrotron X-ray diffraction and electron microscopy

Synchrotron X-ray diffraction and transmission electron microscopy (TEM) were applied to quantitatively characterize the average particle size and size distribution of free-standing TiB{sub 2} particles and TiB{sub 2} particles in an in-situ grown Al–TiB{sub 2} composite. The detailed evaluations were carried out by X-ray line profile analysis using the restricted moment method and multiple whole profile fitting procedure (MWP). Both numerical methods indicate that the formed TiB{sub 2} particles are well crystallized and free of crystal defects. The average particle size determined from different Bragg reflections by the restricted moment method ranges between 25 and 55 nm, where the smallest particle size is determined using the 110 reflection suggesting the highest lateral-growth velocity of (110) facets. The MWP method has shown that the in-situ grown TiB{sub 2} particles have a very low dislocation density (~ 10{sup 11} m{sup −} {sup 2}) and their size distribution can be described by a log-normal distribution. Good agreement was found between the results obtained from the restricted moment and MWP methods, which was further confirmed by TEM. - Highlights: • Accurate quantitative characterization of in-situ grown T{sub i}B{sub 2} particles has been achieved. • Particle size anisotropy was revealed indicating 110 facets being largest during T{sub i}B{sub 2} growth. • A wide size distribution was observed for T{sub i}B{sub 2} particles with a dominant size smaller than 100 nm.

36 MATERIALS SCIENCE↗

NASA NTRS1994

Shape, size, and distribution of magnetic particles in Bjurbole chondrules

Chondrules from the Bjurbole chondritic meteorite (L4) exhibit saturation remanence magnetization (SIRM) values which vary over three orders of magnitude. REM values (Natural Remanence Magnetization/SIRM) for Allende (C3V) and Chainpur (LL3) are less than 0.01 but in Bjurbole some chondrules were found to have REM values greater than 0.1 with several greater than 0.2. REM values greater than 0.1 are abnormal and cannot be acquired during weak field cooling. If exposure to a strong field (whatever the source) during the chondrules' history is responsible for the high REM values, was such history associated with a different processing which might have resulted in different shape, size, and distribution of metal particles compared to chondrules having REM values of less than 0.01? Furthermore, magnetic hysteresis results show a broad range of magnetic hardness and other intrinsic magnetic properties. These features must be related to (1) size and amount of metal; and (2) properties of, and amount of, tetrataenite in the chondrules (all chondrules thus far subjected to thermomagnetic analysis show the presence of tetrataenite). A scanning electron microscopy (SEM) study is underway to determine the relationship between the shape, size, and distribution of metal particles within individual chondrules and the magnetic properties of these chondrules. Results from the SEM study in conjunction with magnetic property data may also help to discern effects from possible lightning strikes in the nebula prior to incorporation of the chondrules into the parent body.

Nava, David F.↗

DOE OSTI2014

Silica Supported Ceria Nanoparticles: A Hybrid Nanostructure To Increase Stability And Surface Reactivity Of Nano-crystalline Ceria

The mixed oxidation state (3+/4+) of ceria nanoparticles of smaller sizes make them attractive materials for their catalytic antioxidant biological properties. However the unmodified smaller ceria nanoparticles are limited in their use due to particles agglomeration and reduced surface chemical reactivity in the solutions used to disperse the nanoparticles. This work describes an effort to stabilize small ceria nanoparticles, retaining their desired activity, on a larger stable silica support. The ceria nanoparticles attached to silica was synthesized by a solution synthesis technique in which the surface functional groups of silica nanoparticles were found to be essential for the formation of smaller ceria nanoparticles. The surface chemical and vibrational spectroscopy analysis revealed cerium–silicate (Ce-O-Si) covalent bond linkage between silica and cerium oxide nanoparticles. The colloidal properties (agglomerate particle size and suspension stability) of ceria attached to silica was significantly improved due to inherent physico-chemical characteristics of silica against random collision and gravitation settling as opposed to unmodified ceria nanoparticles in solution. The bio-catalytic activity of ceria nanoparticles in the 3+ oxidation state was not found to be limited by attachment to the silica support as measured by free radical scavenging activity in different biological media conditions.

Environmental Molecular Sciences Laboratory↗

DOE OSTI2016

Link between microstructure and tritiated water diffusivity in mortars: Impact of aggregates

The present study aims to investigate the influence of microstructure, particularly the effect of aggregates content and interfacial transition zone (ITZ), on tritiated water (HTO) diffusivity in mortars. To this end, three different series of mortars were prepared and HTO diffusion tests were conducted. Variables are water-to-cement ratio, sand volume fractions, and particle size distribution. In parallel, the microstructure of these materials was characterized by water porosimetry, mercury porosimetry, and by backscattered electron microscopy associated to images analysis. It was observed that at low sand content (0%–50%), diffusion properties of mortars are dominated by aggregates dilution effect. Beyond 50% of standard sand, other effects related to the large number of sand grains appear, such as air voids and porous areas mainly due to the difficulty of obtaining well-compacted materials.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Spherical Aberrations - Final Focus and Solenoid Scans

Conclusions: Spherical aberrations in solenoids are unavoidable and problematic whenever the beam is focused; It may be possible to include a spherical aberration correction to the analysis of a solenoid scan in the manner described above although more accurate 2D PIC models should be studied to determine the accuracy of the very simple model used above. This correction would have to be iterated as the beam size in the solenoid is iterated; A quadrupole triplet final focus would not have aberrations (preliminary analysis shows improvement in spot size, very difficult to tune).

43 PARTICLE ACCELERATORS↗

DOE OSTI2019

Multidrug Core–Shell Bead: A System for Bacterial Infection Treatment in Fish

This study was developed to improve the durability and bioavailability of polymer matrix containing the antibacterial agent’s bacitracin (BAC), berberine (BER) and sodium nitroprusside (SNP), an ionotropic gelation method was successfully applied to prepare alginate/chitosan core–shell beads. The structure and properties of different core–shell beads were characterized by scanning electron microscopy (SEM), zeta potential, Fourier transform infrared spectroscopy (FTIR), thermal analysis (DSC), swelling tests, bioadhesive assay, release kinetic profile and antibacterial/antibacteriostatic activity in bacterial model. The morphology of beads was investigated by SEM, display relatively spherical shape and revealed rough surface was also observed the appearance of cracks probably caused by partial collapsing of the polymer network during drying. The diameter means particle size observed was around 1.04 ± 0.13 mm, the particles showed a neutral value, around + 0.305 mV. Using UV–Vis technique was observed a high entrapment efficiency of compounds BAC, BER and SNP (> 95%) in the alginate/chitosan core–shell beads. As demonstrated, there is increase in the swelling degree in pH 6.2. The drug release profile showed a pH-dependent release kinetics. At pH 5.0 the most suitable kinetic model is Higuchi, at pH 6.2 a zero-order model is observed, while at pH 7.4 the Korsmeyer–Peppas model present a good fit. The presence of compounds on beads was confirmed using FTIR analyses, and the results indicated that there is no interaction between drugs and vehicle used in the formulation. We can consider after DSC analysis that beads containing BAC, BER and SNP are thermally more stable than separate formulations having the characteristics required for application at room temperature. The release system produced has physical characteristics that allow the storage of the drugs for long periods of time maintaining their chemical and pharmacological properties unchanged. The percentage of adhesion displayed value of 66%, that indicates the improvement in adherence time on the absorbing surfaces to improves drug bioavailability and effectiveness of compounds. In this study is displayed the additive effect between BAC, BER and SNP shown the potential application of compound combinations as an efficient, novel therapeutic tool for antibiotic-resistant bacterial infections. These results indicate that the proposed strategy improves drug bioavailability and effectiveness of compounds in the treatment of fish.

36 MATERIALS SCIENCE↗

NASA NTRS1992

Study of cosmic dust particles on board LDEF: The FRECOPA experiments AO138-1 and AO138-2

Two experiments, within the French Cooperative Payload (FRECOPA) and devoted to the detection of cosmic dust, were flown on the LDEF. A variety of sensors and collecting devices have made possible the study of impact processes on materials of technological interest. Preliminary examination of hypervelocity impact features gives valuable data on size distribution and nature of interplanetary dust particles in low earth orbit, within the 0.5 to 300 micrometer size range. Most of the events detected on the trailing face of LDEF are expected to be the result of impacts of meteoritic particles only. So far, chemical analysis of craters by EDS clearly shows evidence of elements (Na, Mg, Si, S, Ca, and Fe) consistent with cosmic origin. Systematic occurrence of C and O in crater residues is an important result, to be compared with the existence of CHON particles detected in P-Halley comet nucleus. Crater size distribution is in good agreement with results from other dust experiments flown on LDEF. However, no crater smaller than 1.5 micron was observed, thus suggesting a cutoff in the near earth particle distribution. Possible origin and orbital evolution of micrometeoroids is discussed.

Mandeville, J. C.↗

DOE OSTI2019

Systematic Mapping of Binary Nanocrystal Superlattices: The Role of Topology in Phase Selection

The self-assembly of two sizes of spherical nanocrystals has revealed a surprisingly diverse library of structures. To date, at least 15 distinct binary nanocrystal superlattice (BNSL) structures have been identified. The stability of these binary phases cannot be fully explained using the traditional conceptual framework treating the assembly process as entropy-driven crystallization of rigid spherical particles. Such deviation from hard sphere behavior may be explained by the soft and deformable layer of ligands that envelops the nanocrystals, which contributes significantly to the overall size and shape of assembling particles. In this work, we describe a set of experiments designed to elucidate the role of the ligand corona in shaping the thermodynamics and kinetics of BNSL assembly. Using hydrocarbon-capped Au and PbS nanocrystals as a model binary system, we systematically tuned the core radius ( R ) and ligand chain length ( L ) of particles and subsequently assembled them into binary superlattices. The resulting database of binary structures enabled a detailed analysis of the role of effective nanocrystal size ratio, as well as softness expressed as L/R , in directing the assembly of binary structures. This catalog of superlattices allowed us to not only study the frequency of different phases but to also systematically measure the geometric parameters of the BNSLs. Furthermore, this analysis allowed us to evaluate new theoretical models treating the cocrystallization of deformable spheres and to formulate new hypotheses about the factors affecting the nucleation and growth of the binary superlattices. Among other insights, our results suggest that the relative abundance of the binary phases observed may be explained not only by considerations of thermodynamic stability, but also by a postulated preordering of the binary fluid into local structures with icosahedral or polytetrahedral symmetry prior to nucleation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Multi-modal chemical characterization of highly viscous submicrometer organic particles

Distinguishing highly viscous organic particles within complex mixtures of atmospheric aerosol and accurate descriptions of their composition, size distributions, and mixing states are challenges at the forefront of aerosol measurement science and technology. Here, we present results obtained from complementary single-particle measurement techniques employed for the in-depth characterization of highly viscous particles. In this study, we demonstrate advantages and synergy of this multi-modal particle characterization approach based on the analysis of individual viscous particles formed in the air-discharged waste produced by a common sewer pipe rehabilitation technology. Using oil immersion flow microscopy, we investigate particle size distributions and morphology of colloidal components present in field-collected aqueous waste condensates. We compare these results with corresponding measurements of viscous particles formed in drying droplets of the aerosolized discharged waste. The colloidal components and viscous particles were found to be approximately 10 µm and 0.5 µm, respectively. The aerosolized viscous particles exhibited a spherical morphology, while the colloidal particles appeared noticeably fractal, resembling fragments of a cured composite material. Chemical imaging of the viscous particles collected on substrates was performed using scanning electron microscopy and soft X-ray spectro-microscopy techniques. Through these methods, comprehensive description of these particles emerged, confirming their high solid-like viscosity, wide-ranging sizes, diverse carbon speciation with high degrees of oxygenation, and high organic volume fractions. The aerosolized viscous particles were further characterized using high-throughput single particle mass spectrometry. This technique provides real-time measurements of composition, size, and morphological metrics for large numbers of individual particles, enabling the identification of their distinct mass spectrometric signatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1976

Results of the asteroid-meteoroid particle experiment on Pioneer 11

The Asteroid-Meteoroid Detector, an electro-optical instrument that detects and measures particles in space by sensing the sunlight reflected from them, is part of the payload of both the Pioneer 10 and 11 spacecraft. The Pioneer 11 instrument is essentially identical to that on Pioneer 10, with some minor modifications. Reduction of the Pioneer 11 data was complicated by the failure of one of the four sensor channels at about 1.1 AU from the sun. Detailed analysis yielded 51 events between 1.0 and 3.5 AU, which were used to determine the particle concentration distribution in that region of space. Weighted curve-fitting of the results shows agreement with the concentrations derived from Pioneer 10 to within about a factor of two. As with the Pioneer 10 results, the exponent of the size dependency varies from about -1.7 for 100-micron radius particles to about -3.2 for 10-cm bodies. The instrument, its operation, and the method of data analysis are reviewed.

Soberman, R. K.↗

DOE OSTI2015

A discrete element based simulation framework to investigate particulate spray deposition processes

This work presents a computer simulation framework based on discrete element method to analyze manufacturing processes that comprise a loosely flowing stream of particles in a carrier fluid being deposited on a target surface. The individual particulate dynamics under the combined action of particle collisions, fluid–particle interactions, particle–surface contact and adhesive interactions is simulated, and aggregated to obtain global system behavior. A model for deposition which incorporates the effect of surface energy, impact velocity and particle size, is developed. The fluid–particle interaction is modeled using appropriate spray nozzle gas velocity distributions and a one-way coupling between the phases. It is found that the particle response times and the release velocity distribution of particles have a combined effect on inter-particle collisions during the flow along the spray. It is also found that resolution of the particulate collisions close to the target surface plays an important role in characterizing the trends in the deposit pattern. Analysis of the deposit pattern using metrics defined from the particle distribution on the target surface is provided to characterize the deposition efficiency, deposit size, and scatter due to collisions.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2016

Quantitative characterization of material surface — Application to Ni + Mo electrolytic composite coatings

A new approach to numerical analysis of maps of material surface has been proposed and discussed in detail. It was concluded that the roughness factor RF and the root mean square roughness S{sub q} show a saturation effect with increasing size of the analysed maps what allows determining the optimal map dimension representative of the examined material. A quantitative method of determining predominant direction of the surface texture based on the power spectral density function is also proposed and discussed. The elaborated method was applied in surface analysis of Ni + Mo composite coatings. It was shown that co-deposition of molybdenum particles in nickel matrix leads to an increase in surface roughness. In addition, a decrease in size of the embedded Mo particles in Ni matrix causes an increase of both the surface roughness and the surface texture. It was also stated that the relation between the roughness factor and the double layer capacitance C{sub dl} of the studied coatings is linear and allows determining the double layer capacitance of the smooth nickel electrode. - Highlights: •Optimization of the procedure for the scanning of the material surface •Quantitative determination of the surface roughness and texture intensity •Proposition of the parameter describing privileged direction of the surface texture •Determination of the double layer capacitance of the smooth electrode.

36 MATERIALS SCIENCE↗

DOE OSTI2021

In-situ magnetic alignment model for additive manufacturing of anisotropic bonded magnets

In this work, we report a mathematical framework which predicts the degree of alignment (DoA) in an in-situ aligned additively manufactured 3D printed bonded magnets. A multiphysics model is developed which couples the harmonious interactions of magnetic particles in a viscous flowing polymer under the presence of an external magnetic field. The hydrodynamic fluid-particle interaction is paired with the magnetophoretic force to predict the particle trajectory and distribution during extrusion through a 3D printer nozzle. Succeeding the force balance, a magnetohydrodynamic torque equilibrium analysis is performed to predict the net-orientation of the magnetic particles as a function of the applied field strength, viscous forces, and particle-to-particle interactions (P2P). Experimental validation of the DoA predictions is performed using 65 vol% Nd-Fe-B+Sm-Fe-N in Nylon12 (DoA exp = 0.620 and DoA theory = 0.686) and 15 vol% Sm-Co in PLA (DoA exp = 0.830 and DoA theory = 0.863). A parametric analysis is performed to analyze the effect of operating and design parameters like alignment field strength, magnetic loading fraction, extrusion load, and particle size. The model predicts a competing behavior between particle-fluid and particle-particle interactions under the presence of an applied field. Lastly, the model provides a framework to efficiently predict the DoA in tandem with a functionalized-magnetic 3D printer and allows the user to adjust the operating parameters according to the desired DoA.

36 MATERIALS SCIENCE↗

NASA NTRS1992

A case of type I polar stratospheric cloud formation by heterogeneous nucleation

The NASA ER-2 aircraft flew on January 24, 1989, from Stavanger to Spitsbergen, Norway, at the 430-440 K potential temperature surface (19.2-19.8 km pressure altitude). Aerosols were sampled continuously by an optical particle counter (PMS-FSSP300) for concentration and size analyses, and during five 10-min intervals by four wire and one replicator impactor for concentration, size, composition, and phase analysis. During sampling, the air saturation of H2O with respect to ice changed from 20 to 100 percent, and of HNO3 with respect to nitric acid trihydrate (NAT) from subsaturation to supersaturation. Data from both instruments indicate a condensation of hydrochloric acid and, later, nitric acid on the background aerosol particles as the ambient temperature decreases along the flight track. This heterogeneous nucleation mechanism generates type I polar stratospheric cloud particles of 10-fold enhanced optical depth, which could play a role in stratospheric ozone depletion.

Pueschel, R. F.↗

DOE OSTI2016

A mobile system for a comprehensive online-characterization of nanoparticle aggregates based on wide-angle light scattering and laser-induced incandescence

A mobile demonstrator for the comprehensive online-characterization of gas-borne nanoparticle aggregates is presented. Two optical measurement techniques are combined, both utilizing a pulsed Nd:YAG laser as light source. Aggregate size and fractal dimension are measured by Wide-Angle Light Scattering (WALS). An ellipsoidal mirror images elastically scattered light from scattering angles between 10° and 165° onto a CCD-camera chip resulting in an almost complete scattering diagram with high angular resolution. Primary particle size and volume fraction are measured by time-resolved Laser-Induced Incandescence (TiRe-LII). Here, particles are heated up to about 3000 K by the short laser pulse, the enhanced thermal radiation signal is detected with gated photomultiplier tubes. Analysis of the signal decay time and maximum LII-signal allows for the determination of primary particle diameter and volume fraction. The performance of the system is demonstrated by combined measurements on soot nanoparticle aggregates from a soot aerosol generator. Particle and aggregate sizes are varied by using different equivalence ratios of the combustion in the generator. Soot volume fraction can be adjusted by different levels of dilution with air. Online-measurements were carried out demonstrating the favorable performance of the system and the potential for industrial applications such as process control and product development. The particle properties obtained are confirmed through transmission electron microscopy analysis on representative samples.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Nanoparticle Size and Coating Chemistry Control Foliar Uptake Pathways, Translocation, and Leaf-to-Rhizosphere Transport in Wheat

Nano enabled foliar-applied agrochemicals can potentially be safer and more efficient than conventional products. However,limited understanding about how nanoparticle properties influence their interactions with plant leaves, uptake, translocation through the mesophyll to the vasculature, and transport to the rest of the plant prevents rational design. This study used a combination of Auquantification and spatial analysis to investigate how size (3, 10, or50 nm) and coating chemistry (PVP versus citrate) of gold nano-particles (AuNPs) influence these processes. Following wheat foliar exposure to AuNPs suspensions (~280 ng per plant), adhesion on the leaf surface was increased for smaller sizes, and PVP-AuNPs compared to citrate-AuNPs. After 2 weeks, there was incomplete uptake of citrate-AuNPs with some AuNPs remaining on the outside of the cuticle layer. However, the fraction of citrate-AuNPs that had entered the leaf was translocated efficiently tothe plant vasculature. In contrast, for similar sizes, virtually all of the PVP-AuNPs crossed the cuticle layer after 2 weeks,but its transport through the mesophyll cells was lower. As a consequence of PVP-AuNP accumulation in the leaf mesophyll, wheat photosynthesis was impaired. Regardless of their coating and sizes, the majority of the transported AuNPs accumulated in younger shoots (10-30%) and in roots (10-25%), and 5-15% of the NPs <50 nm were exuded into the rhizosphere soil. A greater fraction of larger sizes AuNPs (presenting lowerζpotentials) was transported to the roots. The key hypotheses about the NPs physical-chemical and plant physiology parameters that may matter to predict leaf-to-rhizosphere transport are also discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗