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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Microstructure and nanoindentation analysis of Mg-SiC nanocomposite powders synthesized by mechanical milling

Highlights: • Mechanical milling as an effective solution to reach a homogeneous distribution of SiC nanoparticles up to 10 vol% in Mg matrix • No deformation twinning in the nanostructured Mg matrix even after the severe plastic deformation and hard SiC nanoparticles up to 10 vol%. • Significant enhancement of nanohardness and reduced elastic modulus in the milled nanocomposite powders - Abstract: Mixtures of magnesium powder and SiC nanoparticles at various volume fractions were mechanically milled to produce nanocrystalline Mg-SiC nanocomposites. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were utilized to characterize the microstructure of the milled powders. The microstructural evidences revealed that mechanical milling is a proper method to achieve a uniform distribution of the SiC nanoparticles, even up to 10% in the Mg matrix. Based on the results, higher volume fraction of the SiC nanoparticles raise the value of measured microstrain and reduce the crystallite size of the Mg matrix. The TEM results pointed to the fact that no deformation twinning takes place in the nanostructured Mg matrix even after severe plastic deformation through mechanical milling and the presence of hard SiC nanoparticles up to 10 vol%. The effects of nanoparticle volume fraction on mechanical properties of the milled Mg-SiC nanocomposites were evaluated using nanoindentation tests. The results clearly showed a significant enhancement of nanohardness and reduced elastic modulus in the milled powders compared to that of the reference material namely as-received pure magnesium. It was found that the SiC nanoparticles (even up to 10 vol%), well distributed in the magnesium matrix, remarkably improve the reduced elastic modulus and nanohardness of the nanocomposite powders.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2026

Integrating Carbon Capture, Utilization, & Sequestration into Chemical Pulp Mills

The U.S. pulp and paper industry presents a unique and largely untapped opportunity for large- scale carbon dioxide removal (CDR). Unlike most industrial sectors, pulp mills rely heavily on biomass, meaning that much of their carbon emissions originate from atmospheric CO₂ that was recently captured by plants. If this biogenic CO₂ can be captured and permanently stored, pulp mills can be transformed from carbon emitters into net carbon removal facilities. This project was motivated by that opportunity and aimed to develop and evaluate integrated, low-cost strategies for capturing, utilizing, and sequestering CO₂ within existing chemical pulping operations. The scope of this work focused on four complementary innovations designed to integrate seamlessly into kraft pulp mill infrastructure: (1) in situ CO₂ capture within the recovery cycle, (2) oxy-fuel retrofitting of the rotary lime kiln to produce a high-purity CO₂ stream, (3) ex situ CO₂ capture and mineralization using pulp mill residues (dregs, grits, and lime mud), and (4) beneficial reuse of these residues as mineral carbonate fertilizers. The project combined process modeling, laboratory experimentation, life cycle assessment (LCA), and field trials to evaluate the technical feasibility, economic viability, and environmental impact of these approaches. The results demonstrate that pulp mills can serve as effective platforms for carbon removal when equipped with integrated carbon capture systems. Process modeling showed that combining sodium spiking with oxy-fuel calcination significantly enhances CO₂ capture efficiency while reducing costs by up to 31% compared to conventional configurations. Experimental work further revealed that calcination behavior in high-CO₂ environments differs substantially from traditional systems, leading to the development of a new kinetic model that predicts reaction rates under these conditions. This model provides essential design guidance for next-generation decarbonized lime kilns. In parallel, the project demonstrated that alkaline mineral residues generated during pulping operations can be repurposed as a sustainable alternative to agricultural lime. Across a wide range of soils in the southeastern United States, these materials performed equivalently to commercial lime in adjusting soil pH while offering lower greenhouse gas emissions and reduced cost. Field and greenhouse studies confirmed that crop and tree growth responses were comparable, supporting their viability as a drop-in replacement. This co-product pathway provides a practical utilization strategy that offsets costs and improves overall system economics. A major contribution of this project is the first comprehensive life cycle assessment of carbon removal in pulp and paper systems across multiple system boundaries. Results show that retrofitted mills can achieve carbon removal efficiencies ranging from 12% to 92%, depending on how the system is defined. This finding highlights a critical issue in carbon accounting: reported performance is highly sensitive to methodological choices. By explicitly quantifying these differences, this work provides valuable guidance for policymakers, carbon registries, and project developers working to standardize carbon removal metrics. From a commercialization perspective, the technologies investigated in this project are well- aligned with existing industrial infrastructure, minimizing the need for entirely new facilities. 3 DE-EE0009413 Industry engagement throughout the project—including collaboration with pulp and paper companies, equipment manufacturers, and carbon removal developers—has accelerated the transition from research to deployment. Notably, a commercial developer is actively pursuing carbon capture projects at pulp mills in the southeastern United States and has cited this research as a contributing foundation. The emergence of voluntary carbon markets and long-term offtake agreements further strengthens the business case for implementation. The broader public benefits of this work are significant. By enabling large-scale carbon removal using existing industrial systems, this approach offers a near-term pathway to reduce atmospheric CO₂ concentrations while supporting domestic manufacturing and rural economies. The reuse of industrial residues as fertilizers reduces reliance on mined materials, lowers costs for farmers, and decreases environmental impacts associated with conventional lime production. In addition, the project has supported workforce development by training graduate students and researchers in carbon capture technologies, helping to build capacity in a critical area of national interest. In conclusion, this project demonstrates that integrated carbon capture, utilization, and sequestration in pulp mills is both technically feasible and economically promising. By combining process innovation, experimental validation, and systems-level analysis, the work advances the understanding of how biomass-based industries can contribute to climate mitigation. The findings provide a strong foundation for commercial deployment and offer a scalable solution for transforming a major U.S. industry into a source of durable carbon removal.

09 BIOMASS FUELS↗
NASA NTRS2006

A Low Noise, Microprocessor-Controlled, Internally Digitizing Rotating-Vane Electric Field Mill for Airborne Platforms

This paper reports on a new generation of aircraft-based rotating-vane style electric field mills designed and built at NASA's Marshall Spaceflight Center. The mills have individual microprocessors that digitize the electric field signal at the mill and respond to commands from the data system computer. The mills are very sensitive (1 V/m per bit), have a wide dynamic range (115 dB), and are very low noise (+/-1 LSB). Mounted on an aircraft, these mills can measure fields from +/-1 V/m to +/-500 kV/m. Once-per-second commanding from the data collection computer to each mill allows for precise timing and synchronization. The mills can also be commanded to execute a self-calibration in flight, which is done periodically to monitor the status and health of each mill.

Bateman, M. G.↗
DOE OSTI2010

Coercivity and superparamagnetic evolution of high energy ball milled (HEBM) bulk CoFe{sub 2}O{sub 4} material

Ball milling (BM) of bulk CoFe{sub 2}O{sub 4} powder material carried out in order to study its structural stability and attendant property changes with respect to coercivity enhancements and superparamagnetic behaviors, showed that drastic crystallite size reduction occurred within the first 1 h of ball milling. Crystallite size dropped from 74 nm for the as-received material to a value of 11.6 nm for 600 min of ball milling. Combined X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses confirmed crystallite size reduction with corresponding increase in interparticle agglomeration/pores with increasing milling time. The maximum coercivity of 0.46 T and the crystallite size of 15.6 nm were recorded with 20 min, while peak residual strain of 0.0066 mm/mm was for 180 min of BM. Material with peak coercivity value did not have peak residual strain, or minimum crystallite size, thereby suggesting that other structural defects contributed to coercivity enhancement. The saturation magnetization (M{sub s}) value decreased continuously with increasing milling time, while remanence magnetization (M{sub r}) and coercivity decreased with increasing BM time, after an initial increase. Moessbauer spectroscopy (MS) measurements confirmed both particle size distribution and decomposition/disordering of the material together with superparamagnetism as BM time increased. The degree of inversion ranged from 41% to 71.7% at different milled states from Moessbauer spectroscopy. The internal magnetic fields of the Fe sites associated with the tetrahedral and octahedral sites were 507.4 kOe and 492 kOe respectively in the unmilled state, while 484 kOe and 468.5 kOe in the 600 min milled state correspondingly.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Powder properties of hydrogenated ball-milled graphite

Ball milling is an effective way of producing defective and nanostructured graphite. In this work, the hydrogen storage properties of graphite, ball-milled in a tungsten carbide milling pot under 3 bar hydrogen for various times (0–40 h), were investigated by TGA-Mass Spectrometry, XRD, SEM and laser diffraction particle size analysis. For the conditions used in this study, 10 h is the optimum milling time resulting in desorption of 5.5 wt% hydrogen upon heating under argon to 990 °C. After milling for 40 h, the graphite became significantly more disordered, and the amount of desorbed hydrogen decreased. After milling up to 10 h, the BET surface area increased while particle size decreased; however, there is no apparent correlation between these parameters, and the hydrogen storage properties of the hydrogenated ball-milled graphite.

36 MATERIALS SCIENCE↗
DOE OSTI2017

An environmentally friendly ball milling process for recovery of valuable metals from e-waste scraps

Highlights: • A new ball milling process was successfully developed for recovery of metals from e-waste. • The process produce soluble metallic compound with dry ball milling and benefits the leaching process. • Precious metals were successfully separated from base metals during the process. • Mechanism of the mechanochemical reactions was proposed. - Abstract: The present study reports a mechanochemical (MC) process for effective recovery of copper (Cu) and precious metals (i.e. Pd and Ag) from e-waste scraps. Results indicated that the mixture of K{sub 2}S{sub 2}O{sub 8} and NaCl (abbreviated as K{sub 2}S{sub 2}O{sub 8}/NaCl hereafter) was the most effective co-milling reagents in terms of high recovery rate. After co-milling with K{sub 2}S{sub 2}O{sub 8}/NaCl, soluble metallic compounds were produced and consequently benefit the subsequent leaching process. 99.9% of Cu and 95.5% of Pd in the e-waste particles could be recovered in 0.5 mol/L diluted HCl in 15 min. Ag was concentrated in the leaching residue as AgCl and then recovered in 1 mol/L NH{sub 3} solution. XRD and XPS analysis indicated that elemental metals in the raw materials were transformed into their corresponding oxidation state during ball milling process at low temperature, implying that solid–solid phase reactions is the reaction mechanism. Based on the results and thermodynamic parameters of the probable reactions, possible reaction pathways during ball milling were proposed. Suggestion on category of e-waste for ball milling process was put forward according to the experiment results. The designed metal recovery process of this study has the advantages of highly recovery rate and quick leaching speed. Thus, this study offers a promising and environmentally friendly method for recovering valuable metals from e-waste.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Effects of Ball Milling on the Electrochemical Capacity and Interfacial Stability of Li 2 MnO 3 Cathode Materials

The cycling mechanism of Li 2 MnO 3 cathode materials synthesized by conventional solid-state methods at high temperatures (800-900 °C) has been intensively investigated. Previous studies showed that CO 2 and O 2 gas evolution accounts for most of the charge capacity, followed by some Mn reduction during discharge. In this work, we analyze the effects of ball milling on the structure, surface contaminant, and electrochemical capacity of Li 2 MnO 3 cathode material, with or without a graphitic fluoride (C-F) additive. At the same time, C-F is added to form a protective coating layer that reduces unwanted reactions with the electrolyte during later electrochemical cycling. We find that the C-F ball-milled material shows Li 2 MnO 3 /LiMnO 2 composite phases, while the purely ball-milled material shows a single Li 2 MnO 3 phase. Furthermore, we characterize surface species and gas evolution during the first cycle, which reveals the decomposition of Li 2 CO 3 and the carbonate electrolyte during the first charge, especially during the high potential region (>4.4 V), and the electrochemical reduction of only a small fraction of the evolved gas on the first discharge (<2.75 V). The appearance further demonstrates the repetitive nature of this process during charge and disappearance during discharge of Mn 2p 3/2 X-ray photoelectron spectroscopy (XPS) spectra signals during the first two cycles. These processes result in first discharge specific capacities of only 155 and 170 mAh/g after first charge specific capacities of 210 and 320 mAh/g for the pure ball-milled and ball-milled with C-F materials, respectively. These studies demonstrate the interfacial instability introduced by ball milling. However, the electrochemical capacity is significantly increased, necessitating further investigation to determine whether ball milling can activate Mn-containing cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2014

Energy Efficiency Feasibility Study and Resulting Plan for the Bay Mills Indian Community

In 2011 the Inter-Tribal Council of Michigan, Inc. was awarded an Energy Efficiency Development and Deployment in Indian Country grant from the U.S. Department of Energy’s Tribal Energy Program. This grant aimed to study select Bay Mills Indian Community community/government buildings to determine what is required to reduce each building’s energy consumption by 30%. The Bay Mills Indian Community (BMIC) buildings with the largest expected energy use were selected for this study and included the Bay Mills Ellen Marshall Health Center building, Bay Mills Indian Community Administration Building, Bay Mills Community College main campus, Bay Mills Charter School and the Waishkey Community Center buildings. These five sites are the largest energy consuming Community buildings and comprised the study area of this project titled “Energy Efficiency Feasibility Study and Resulting Plan for the Bay Mills Indian Community”. The end objective of this study, plan and the Tribe is to reduce the energy consumption at the Community’s most energy intensive buildings that will, in turn, reduce emissions at the source of energy production, reduce energy expenditures, create long lasting energy conscious practices and positively affect the quality of the natural environment. This project’s feasibility study and resulting plan is intended to act as a guide to the Community’s first step towards planned energy management within its buildings/facilities. It aims to reduce energy consumption by 30% or greater within the subject facilities with an emphasis on energy conservation and efficiency. The energy audits and related power consumption analyses conducted for this study revealed numerous significant energy conservation and efficiency opportunities for all of the subject sites/buildings. In addition, many of the energy conservation measures require no cost and serve to help balance other measures requiring capital investment. Reoccurring deficiencies relating to heating, cooling, thermostat setting inefficiencies, powering computers, lighting, items linked to weatherization and numerous other items were encountered that can be mitigated with the energy conservation measures developed and specified during the course of this project.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
DOE OSTI2026

Thermoreflectance Detection of Point Defects Resulting from Focused Ion Beam Milling

Focused ion beam (FIB) milling is a commonly used tool for nanoscale material processing, such as for transmission electron microscopy (TEM) sample preparation, or the creation of fiducial markers prior to other processes and measurements. During milling, a high energy ion beam is used to remove material via sputtering. The expelled target material may return to the sample surface however, affecting subsequent measurements. Beam spreading or irradiation due to neutral gallium may also irradiate a larger area than intended. Extensive research has explored the effects of FIB milling on the prepared TEM sample, but few have looked at the effects of milling on the properties of the sample surrounding the milled region. We use multiple pump-probe laser-based techniques (time domain thermoreflectance and steady-state thermoreflectance) to measure the spatial extent of FIB-induced surface/subsurface changes on a series of silicon wafers milled at multiple currents and doses. We supplement these measurements with high-resolution scanning transmission electron microscopy, energy dispersive X-ray spectroscopy, stylus profilometry, and time-of-flight secondary ion mass spectroscopy. We find a sample surface affected by the FIB up to 1 mm from where milling occurred, with a notable dependence on the ion beam current. We also note remarkably high sensitivity to surface defects using the thermoreflectance metrologies, including detection where other measurements failed.

defects↗
DOE OSTI2017

Explicit formulae for Yang-Mills-Einstein amplitudes from the double copy

Using the double-copy construction of Yang-Mills-Einstein theories formulated in our earlier work, we obtain compact presentations for single-trace Yang-Mills-Einstein tree amplitudes with up to five external gravitons and an arbitrary number of gluons. These are written as linear combinations of color-ordered Yang-Mills trees, where the coefficients are given by color/kinematics-satisfying numerators in a Yang-Mills + φ 3 theory. The construction outlined in this paper holds in general dimension and extends straightforwardly to supergravity theories. For one, two, and three external gravitons, our expressions give identical or simpler presentations of amplitudes already constructed through string-theory considerations or the scattering equations formalism. Our results are based on color/kinematics duality and gauge invariance, and strongly hint at a recursive structure underlying the single-trace amplitudes with an arbitrary number of gravitons. We also present explicit expressions for all-loop single-graviton Einstein-Yang-Mills amplitudes in terms of Yang-Mills amplitudes and, through gauge invariance, derive new all-loop amplitude relations for Yang-Mills theory.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Study of reaction sequences during MSR synthesis of TiC by controlled ball milling of titanium and graphite

Highlights: • Insights on oxygen-bonded features formed during reactive ball milling • Evolution of off-stoichiometric TiC before ignition • Growth sequence of the TiC manifested as stacks and multilayers • Dual morphology of the MSR reaction product - Abstract: During reactive ball milling of Ti and C, mechanically induced self-propagating reaction (MSR) synthesis of TiC is reported to occur via a process including initial formation of small amounts of TiC prior to exothermic ignition, followed by MSR and the formation of stiochiometric TiC (Dorofeev et al., 2011; Oghenevweta et al., 2016 [1, 2]). However, both the chemical evolution and mechanisms of reaction and growth of TiC both prior to, during and after ignition are not fully understood. This research focuses on fundamental understanding of the reaction sequences during MSR synthesis of TiC from elemental Ti and C (graphite). Magnetically controlled ball milling of stoichiometric (1:1) powder mixtures of titanium (Ti) and graphite (C) was performed under He gas with the exothermic ignition point by determined via in-situ temperature measurement. X-ray diffraction, Scanning Transmission Electron Microscopy (STEM) with electron energy loss spectroscopy (EELS), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS) were employed to interpret the reaction sequences. The reaction sequence involved the following: During milling prior to ignition, severely deformed Ti, spheriodised graphite and amorphous carbon forms, and minor amounts of off-stiochiometric nano-TiC{sub 1−x} crystals. In addition to the formation of TiC{sub 1−x}, XPS revealed the formation of oxide skins coating the surface regions of the milled powders. There is also an evolution towards stiochiometric TiC with increasing milling time. Immediately after ignition, a reacted product comprising a mixture of multi-layer stacks of thin TiC plates form, in addition to a matrix comprising large TiC particles which have been liquid phase sintered under the high local heat of reaction by thin layers of unreacted Ti. MSR occurs via a dual mechanism involving rapid growth of existing TiC, plus nucleation and growth of new TiC. High spatially resolved EELS combined with STEM revealed additional information about the inhomogeneous chemical environment of the milled powders.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis of aluminum nitride powders from a plasma-assisted ball milled precursor through carbothermal reaction

Highlights: • A novel and high efficiency synthesizing AlN powders method combining mechanical ball milling and DBDP has been developed. • The particle size, the crystallite size, the lattice distortion, the morphology of Al{sub 2}O{sub 3} powders, and the AlN conversion rate are investigated and compared under the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP. • The ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermal temperature. - Abstract: In this paper, aluminum nitride (AlN) powers have been produced with a novel and high efficiency method by thermal annealing at 1100–1600 °C of alumina (Al{sub 2}O{sub 3}) powders which were previously ball milled for various time up to 40 h with and without the assistant of dielectric barrier discharge plasma (DBDP). The ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP and the corresponding synthesized AlN powers are characterized by X-ray diffraction, scanning electron microscope, and transmission electron microscopy. From the characteristics of the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP, it can be seen that the ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermal temperature. Meanwhile, the synthesized AlN powders can be known as hexagonal AlN with fine crystal morphology and irregular lump-like structure, and have uniform distribution with the average particle size of about between 500 nm and 1000 nm. This provides an important method for fabricating ultra fine powders and synthesizing nitrogen compounds.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Integrated fluorescence light microscopy-guided cryo-focused ion beam-milling for in situ montage cryo-ET

Cryogenic-electron tomography (cryo-ET) permits the in situ visualization of biological macromolecules at the molecular level. Owing to the variable thickness of cells, tissues and organisms, frozen specimens may need to be thinned by cryo-focused ion beam (FIB) milling to produce thin (<500 nm) cryo-lamellae suitable for cryo-ET. Locating regions of interest remains a challenge because untargeted milling can lead to inadvertent ablation and removal of regions of interest. Correlative light and electron microscopy, combined with cryo-FIB milling, can guide the identification of labeled targets in the cellular milieu. Multiple transfers between cryo-imaging instruments, cumbersome correlation algorithms, limited accuracy and low throughput have hindered the routine adoption of cryo-FIB milling within a multimodal correlative workflow for in situ structural biology. Here, in this study, we present a workflow for 3D correlative cryo-fluorescence light microscopy-FIB-ET that streamlines fluorescence light microscopy-guided FIB milling, improving throughput while preserving both structural and contextual information. The complete integration of hardware and software described here minimizes sample contamination from cross-platform exchanges and greatly enhances the efficiency of 3D targeting in cryo-milling. We then describe procedures for implementing montage parallel array cryo-ET (MPACT), which can be easily adapted to any modern life-science transmission electron microscope. MPACT supports high-throughput cryo-ET acquisitions (10 tilt series in 1.5 h) for structure determination and comprehensive contextual understanding of macromolecules within their native surroundings. A complete session from sample preparation to MPACT data processing takes 5−7 d for an individual experienced in both cryo-EM and cryo-FIB milling.

Yang, Jie E. [Univ. of Wisconsin, Madison, WI (Uni↗
NASA NTRS1986

The milling of pristine and brominated P-100 graphite fibers

Techniques were developed for the ball milling of pristine and brominated P-100 graphite fibers. Because of the lubrication properties of graphite, large ball loads (50 percent by volume) were required. Use of 2-propanol as a milling medium enhanced the efficiency of the process. Milled brominated P-100 fibers had resistivities which were indistinguishable from milled pristine P-100 fibers. Apparent loss of bromine from the brominated fibers suggests that bromine would not be the intercalate of choice in applications where milled fibers of this type are required. Other intercalates which do not degas may be more appropriate for a milled fiber application. These same results, however, do provide evidence that bromine molecules leave the fiber surface when removed from overpressure of bromine. While exploring possible solvent media for milling purposes, it was found that brominated fibers are stable in a wide variety of organic solvents.

Dillehay, M. E.↗
NASA NTRS2003

Analytic Solution to the Problem of Aircraft Electric Field Mill Calibration

It is by no means a simple task to retrieve storm electric fields from an aircraft instrumented with electric field mill sensors. The presence of the aircraft distorts the ambient field in a complicated way. Before retrievals of the storm field can be made, the field mill measurement system must be "calibrated". In other words, a relationship between impressed (i.e., ambient) electric field and mill output must be established. If this relationship can be determined, it is mathematically inverted so that ambient field can be inferred from the mill outputs. Previous studies have primarily focused on linear theories where the relationship between ambient field and mill output is described by a "calibration matrix" M. Each element of the matrix describes how a particular component of the ambient field is enhanced by the aircraft. For example the product M(sub ix), E(sub x), is the contribution of the E(sub x) field to the i(th) mill output. Similarly, net aircraft charge (described by a "charge field component" E(sub q)) contributes an amount M(sub iq)E(sub q) to the output of the i(th) sensor. The central difficulty in obtaining M stems from the fact that the impressed field (E(sub x), E(sub y), E(sub z), E(sub q) is not known but is instead estimated. Typically, the aircraft is flown through a series of roll and pitch maneuvers in fair weather, and the values of the fair weather field and aircraft charge are estimated at each point along the aircraft trajectory. These initial estimates are often highly inadequate, but several investigators have improved the estimates by implementing various (ad hoc) iterative methods. Unfortunately, none of the iterative methods guarantee absolute convergence to correct values (i.e., absolute convergence to correct values has not been rigorously proven). In this work, the mathematical problem is solved directly by analytic means. For m mills installed on an arbitrary aircraft, it is shown that it is possible to solve for a single 2m-vector that provides all other needed variables (i.e., the unknown fair weather field, the unknown aircraft charge, and the unknown matrix M). Numerical tests of the solution, effects of measurement errors, and studies of solution non-uniqueness are ongoing as of this writing.

Koshak, William↗
DOE OSTI2020

Ultra-high aspect ratio pores milled in diamond via laser, ion and electron beam mediated processes

Microfabrication techniques are critical for the rapid prototyping and development of applications for cutting edge materials. Recently diamond has gained considerable interest for quantum photonic, biosensing, inertial confinement fusion and magnetometer applications. In this article, ultra-high aspect ratio milling of diamond micropores by photon, ion and electron based methods is reported. A multiphoton absorption laser ablation approach is revealed to rapidly produce sub-10 μm diameter micropores in diamond with an aspect ratio of 14:1 and a tapered profile at the surface interface. Chemically active, oxygen focused ion beam milling produces high-aspect ratio pores in diamond with an aspect ratio of 65:1 and minimal tapering over the length of the pore, overcoming the physical interaction volume limitations imposed in conventional gallium based focused ion beam milling and laser ablation methods. Oxygen-mediated electron beam induced etching is revealed to negate the limitations imposed by physical sputtering mechanisms utilized in focused ion beam milling via the direct initiation of chemical reactions at the receding surface, producing aspect ratios on the order of 200:1. Numerical simulations reveal the physical basis for the superior aspect-ratio pore milling of the oxygen focused ion beam milling and electron beam induced etching methods. Our results demonstrate direct-write methods for the fabrication of ultra-high aspect micropores in diamond and provide insight into the underlying mechanisms of these physical processes. The three methods demonstrated here can be interchanged for applications based on the desired characteristic aspect ratio and process throughput.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The effect of ink ball milling time on interparticle interactions and ink microstructure and their influence on crack formation in rod-coated catalyst layers

This work investigates the influence of ballmilling (sometimes also referred to as jar roller milling) time on cathode catalyst layer (CL) inks and electrode properties using formulations and coating methods relevant for industrial manufacturing. Four CL inks with the same composition were milled for 24, 48, 72, or 96 h. Rheological investigation of these inks showed a reduction of elastic moduli and steady-shear viscosity with continuous ink milling, which is correlated to a decrease in particle-particle interactions as well as formation of smaller agglomerates. Optical microscopy (OM) analysis of the fabricated electrodes revealed a trend in surface crack formation; formulations milled for 24 h contained the lowest average surface crack area percentages of 0.370% at heavy-duty loadings of ~0.300 mg Pt cm -2 , compared to 2.418% for the ink milled for 96 h. Further characterization of the CL through transmission electron microscopy (TEM) imaging showed a decrease in the mean agglomerate and pore size with milling time. Furthermore, these smaller electrode features were consistent with reduced fracture resistance and, hence, development of larger stresses during drying. Our results highlight the need to consider ink processing as an important component in defect-free CL manufacturing.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2013

On the amorphization behavior and hydrogenation performance of high-energy ball-milled Mg{sub 2}Ni alloys

Amorphous Mg{sub 2}Ni alloy was prepared by high energy ball-milling starting with polycrystalline Mg{sub 2}Ni which was prepared with the help of a metallurgy method by using a SPEX 8000D mill. The microstructural and phase structure characterization of the prepared materials was performed via scanning electron microscopy, transition electron microscope and X-ray diffraction. The thermal stabilities were investigated by differential scanning calorimetry. The apparent activation energies were determined by means of the Kissinger method. The first and second crystallization reactions take place at ∼ 255 °C and ∼ 410 °C, and the corresponding activation energy of crystallization is E{sub a1} = 276.9 and E{sub a2} = 382.4 kJ/mol, respectively. At 3 MPa hydrogen pressure and 250 °C, the hydrogen absorption capacities of crystalline, partially and fully amorphous Mg{sub 2}Ni alloy are 2.0 wt.%, 3.2 wt.% and 3.5 wt.% within 30 min, respectively. - Graphical Abstract: We mainly focus on the amorphization behavior of crystalline Mg{sub 2}Ni alloy in the high energy ball-milling process and the crystallization behavior of the amorphous Mg{sub 2}Ni alloy in a follow-up heating process. The relationship of milling, microstructure and hydrogenation properties is established and explained by models. - Highlights: • Amorphous Mg{sub 2}Ni has been obtained by high energy ball milling the as-cast alloy. • The amorphization behavior of polycrystalline Mg{sub 2}Ni is presented. • The crystallization behavior of the amorphous Mg{sub 2}Ni alloy is illustrated. • Establish the relationship of milling, microstructure and hydrogenation properties.

36 MATERIALS SCIENCE↗