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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Reducing waste of the hydride-dehydride process for U-6 wt% Nb spherical powders through lower impact and targeted milling

The breakdown of solid metal into powder during the hydride-dehydride process is commercially important for the formation of titanium and other metal powders. Typically, the milling of the brittle hydride powder occurs in a ball mill, where milling media impacts powder particles to break them down. The milling media can impact particles that are larger than desired, as desired, or smaller than desired, indiscriminately making all particles smaller. In this work, we investigate how to minimize waste powder production during milling using two different milling methods, planetary ball milling and milling in a sieve shaker (sieve-milling). Both processes yielded similar amounts of 20–75 μm diameter powder (the target size range); however, sieve-milling generated a significantly smaller amount of undersized waste powder. The powders were characterized by X-ray diffraction, SEM/STEM, and magnetic susceptibility. Several differences between ball milling and sieve-milling processes are discussed. We then conclude that the decreased yield of undersized powder in sieve-milling was due to a combination of lower impact energy in sieve-milling, unreacted metallic cores in the hydride flakes, and the ability to mill target particle sizes during sieve-milling. While these results are from the milling of brittle hydride powder, similar methods may be applicable to other brittle powders, including ceramics or salts.

Chemistry↗
DOE OSTI2015

Role of intensive milling in the processing of barium ferrite/magnetite/iron hybrid magnetic nano-composites via partial reduction of barium ferrite

In this research a mixture of barium ferrite and graphite was milled for different periods of time and then heat treated at different temperatures. The effects of milling time and heat treatment temperature on the phase composition, thermal behavior, morphology and magnetic properties of the samples have been investigated using X-ray diffraction, differential thermal analysis, high resolution transmission electron microscopy and vibrating sample magnetometer techniques, respectively. X-ray diffraction results revealed that BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} nanocomposites form after a 20 h milling due to the partial reduction of BaFe{sub 12}O{sub 19}. High resolution transmission electron microscope images of a 40 h milled sample showed agglomerated structure consisting of nanoparticles with a mean particle size of 30 nm. Thermal analysis of the samples via differential thermal analysis indicated that for un-milled samples, heat treatment up to 900 °C did not result in α-Fe formation, while for a 20 h milled sample heat treatment at 700 °C resulted in reduction process progress to the formation of α-Fe. Wustite was disappeared in an X-ray diffraction pattern of a heat treated sample at 850 °C, by increasing the milling time from 20 to 40 h. By increasing the milling time, the structure of heat treated samples becomes magnetically softer due to an increase in saturation magnetization and a decrease in coercivity. Saturation magnetization and coercivity of a sample milled for 20 h and heat treated at 850 °C were 126.3 emu/g and 149.5 Oe which by increasing the milling time to 40 h, alter to 169.1 emu/g and 24.3 Oe, respectively. High coercivity values of milled and heat treated samples were attributed to the nano-scale formed iron particles. - Graphical abstract: Display Omitted - Highlights: • Barium ferrite and graphite were treated mechano-thermally. • Increasing milling time increases reduction progress after heat treatment. • Composites including iron nano-crystals forms by milling and heat treatment. • Shorter milling time results in higher H{sub C} of the milled and heat treated samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Structural, Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Gd{sub 5}Si{sub 2}Ge{sub 2}B{sub 0.05} Alloy

Structural, magnetic and magnetocaloric properties of Gd{sub 5}Si{sub 2}Ge{sub 2}B{sub 0.05} alloy, ball milled for different time intervals in the range of 2–50 h were studied. The x-ray powder diffraction analysis of the alloy prior to milling revealed the presence of mixed orthorhombic and monoclinic phases at room temperature. For a milling duration up to 15 h, the alloy powder displayed crystalline nature. Upon further milling, the alloy powder started to lose the crystallinity and after 50 h of milling, the alloy powder displayed amorphous nature. The average particle size of milled samples was found to decrease with increase in milling time. The saturation magnetization value of the bulk alloy 80 emu/g was found to decrease with increase in milling time due to structural disorder. The transition temperature of the milled alloy powder was found to be around 295 K and the transition was found to become broader with increase in milling time. A maximum isothermal entropy change (ΔS{sub max}) of ∼12 J/kg K was obtained in bulk alloy. For a milling duration of 2 h, a marginal decrease of ΔS{sub max} (∼11 J/kg K) was obtained. Whereas, for higher milling durations, (≥ 15 h) a significant decrease in ΔS{sub max} values were observed. However, the broad operating temperature range of the milled powders can be exploited for magnetic refrigeration applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Synthesis and magnetization studies of nanopowder Fe₇₀Ni₂₀Cr₁₀ alloys prepared by high energy milling

Nanocrystalline Fe{sub 1–x–y}Ni x Cr y (x=20, y=10% in Wt)) alloy samples were prepared by mechanical alloying process. Fe, Ni and Cr elemental powders have been ball milled in a planetary mill for various periods of time, up to 27 h. XRD analysis allowed the determination of the structure of the mixture, the average crystallite size and the lattice parameter as a function of milling time. The complete formation of FeNiCr is observed after 27 h milling. With increasing milling time from 0 to 27 h, it is observed that the lattice parameter increases from 0.3515 to 0.3593 nm as well as an increase of microstrain from 0.15 to 0.40%, whereas the grain size decreases from 48 to 13 nm. Grain morphology of the powders at different formation stages was examined using SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time. - Graphical abstract: Fe₇₀Ni₂₀Cr₁₀ nanopowders were prepared using a planetary ball mill. The structure and microstructure vary with milling time; thereby important modifications of the magnetic properties were observed and discussed. Highlights: • Nanocrystalline Fe₇₀Ni₂₀Cr₁₀ alloy were prepared by the mechanical alloying process. • The complete formation of Fe₇₀Ni₂₀Cr₁₀ is observed after 24 h milling. • With increasing milling time, the grain size decreases, while the strain increases. • The SEM images allowed following the morphology of the materials at different stages. • M s and H C derived from the hysteresis are discussed as a function of milling time.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Fabrication of Al{sub 2}O{sub 3}-20 vol.% Al nanocomposite powders using high energy milling and their sinterability

Highlights: Black-Right-Pointing-Pointer Al{sub 2}O{sub 3}/Al nanocomposite powders were prepared via high energy ball milling. After 20 h milling, the size of Al{sub 2}O{sub 3}-20 vol.% Al nanocomposite particles was in the range of 23-29 nm. A uniform distribution of nanosized Al reinforcement throughout the Al{sub 2}O{sub 3} matrix, coating the particles was successfully obtained. Black-Right-Pointing-Pointer There was no any sign of phase changes during the milling. A competition between the cold welding mechanism and the fracturing mechanism were found during milling and finally the above two mechanisms reached an equilibrium. Black-Right-Pointing-Pointer The highest value of relative density was obtained for the sintered bodies at 1500 Degree-Sign C. Black-Right-Pointing-Pointer The harness of the sintered composite was decreased while the fracture toughness was improved after addition Al into alumina. -- Abstract: In this study, alumina-based matrix nanocomposite powders reinforced with Al particles were fabricated and investigated. The sinterability of the prepared nanocomposite powder at different firing temperature was also conducted. Their mechanical properties in terms of hardness and toughness were tested. Alumina and aluminum powder mixtures were milled in a planetary ball mill for various times up to 30 h in order to produce Al{sub 2}O{sub 3}-20% Al nanocomposite. The phase composition, morphological and microstructural changes during mechanical milling of the nanocomposite particles were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) techniques, respectively. The crystallite size and internal strain were evaluated by XRD patterns using Scherrer methods. A uniform distribution of the Al reinforcement in the Al{sub 2}O{sub 3} matrix was successfully obtained after milling the powders. The results revealed that there was no any sign of phase changes during the milling. The crystal size decreased with the prolongation of milling times, while the internal strain increased. A simple model is presented to illustrate the mechanical alloying of a ductile-brittle component system. A competition between the cold welding mechanism and the fracturing mechanism were found during powder milling and finally the above two mechanisms reached an equilibrium. The maximum relative density was obtained at 1500 Degree-Sign C. The harness of the sintered composite was decreased while the fracture toughness was improved after addition Al into alumina.

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

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Nanocrystalline non-stoichiometric SBT: Effect of milling duration on structural and electrical characteristics

In the present work, nanocrystalline specimens of non-stoichiometric Strontium Bismuth Tantalate (SBT) ferroelectric ceramics were synthesized by mechanical activation process using a high energy planetary ball mill. The powders were milled for different milling durations (5, 10, 20 h) keeping the milling speed fixed at 300 rpm. Microstructural characterizations have been performed using X-ray diffraction, scanning electron microscopy, electron diffraction and transmission electron microscopy. Nanocrystallites with average grain size in the range of 30-50 nm are observed to be formed. Grain size is observed to decrease with increasing milling duration. Detailed dielectric study as a function of temperature has been carried out. It is observed that dielectric constant increases and dielectric loss decreases with increasing milling duration. The observed characteristics have been explained in terms of increased number of grain boundaries due to the reduction of granular size. - Highlights: Black-Right-Pointing-Pointer In the present work nano crystalline non-stoichiometric SBT has been synthesized. Black-Right-Pointing-Pointer The technique involved is mechanical activation (high energy ball milling). Black-Right-Pointing-Pointer The milling duration has been optimized. Black-Right-Pointing-Pointer Sr0.8Bi2.2Ta2O9 milled for 20 hours exhibit enhanced electrical characteristics.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Influence of ball milling on atomic structure and magnetic properties of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} glassy alloy

The influence of ball milling on the atomic structure and magnetic properties of the Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} metallic glass with a high thermal stability and excellent soft magnetic properties has been investigated. After 14 h of milling, the obtained powders were found to consist mainly of an amorphous phase and a small fraction of the (Co,Fe){sub 21}Ta{sub 2}B{sub 6} nanocrystals. The changes in the reduced pair correlation functions suggest noticeable changes in the atomic structure of the amorphous upon ball milling. Furthermore, it has been shown that milling is accompanied by introduction of compressive and dilatational sites in the glassy phase and increasing the fluctuation of the atomic-level hydrostatic stress without affecting the coordination number of the nearest neighbors. Ball milling has decreased the thermal stability and significantly affected the magnetic properties through increasing the saturation magnetization, Curie temperature of the amorphous phase and coercivity. - Highlights: • Ball milling affected the atomic structure of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} metallic glass. • Mechanically-induced crystallization started after 4 h milling. • Milling increased the fluctuation of the atomic-level hydrostatic stress in glass. • Ball milling influenced the thermal stability and magnetic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Phase evolution in carbide dispersion strengthened nanostructured copper composite by high energy ball milling

In this study, high-energy ball milling was applied to synthesis in situ nanostructured copper based composite reinforced with metal carbides. Cu, M (M=W or Ti) and graphite powder mixture were mechanically alloyed for various milling time in a planetary ball mill with composition of Cu-20vol%WC and Cu-20vol%TiC. Then the as-milled powder were compacted at 200 to 400 MPa and sintered in a vacuum furnace at 900 Degree-Sign C. The results of X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy analysis showed that formation of tungsten carbides (W{sub 2}C and WC phases) was observed after sintering of Cu-W-C mixture while TiC precipitated in as-milled powder of Cu-Ti-C composite after 5 h and become amorphous with longer milling. Mechanism of MA explained the cold welding and fracturing event during milling. Cu-W-C system shows fracturing event is more dominant at early stage of milling and W particle still existed after milling up to 60 h. While in Cu-Ti-C system, cold welding is more dominant and all Ti particles dissolved into Cu matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Monticello Mill Tailings Site, Operable Unit lll, Annual Groundwater Report, May 2015 Through April 2016

This report provides the annual analysis of water quality restoration progress, cumulative through April 2016, for Operable Unit (OU) III, surface water and groundwater, of the U.S. Department of Energy (DOE) Office of Legacy Management (LM) Monticello Mill Tailings Site (MMTS). The MMTS is a Comprehensive Environmental Response, Compensation, and Liability Act National Priorities List site located in and near the city of Monticello, San Juan County, Utah. MMTS comprises the 110-acre site of a former uranium- and vanadium-ore-processing mill (mill site) and 1700 acres of surrounding private and municipal property. Milling operations generated 2.5 million cubic yards of waste (tailings) from 1942 to 1960. The tailings were impounded at four locations on the mill site. Inorganic constituents in the tailings drained from the impoundments to contaminate local surface water (Montezuma Creek) and groundwater in the underlying alluvial aquifer. Mill tailings dispersed by wind and water also contaminated properties surrounding and downstream of the mill site. Remedial actions to remove and isolate radiologically contaminated soil, sediment, and debris from the former mill site, Operable Unit I (OU I), and surrounding properties (OU II) were completed in 1999 with the encapsulation of the wastes in an engineered repository located on DOE property 1 mile south of the former mill site. This effectively removed the primary source of groundwater contamination; however, contamination of groundwater and surface water remains within OU III at levels that exceed water quality protection standards. Uranium is the primary contaminant of concern (COC). LM implemented monitored natural attenuation with institutional controls as the OU III remedy in 2004. Because groundwater restoration proceeded more slowly than expected and did not meet performance criteria established in the OU III Record of Decision (June 2004), LM implemented a contingency action in 2009 by an Explanation of Significant Difference to include a pump-and­ treat system using a single extraction well and treatment by zero-valent iron (ex situ treatment system). The contingency action was optimized in 2015 with the installation of8 extraction wells and 16 monitoring wells in a focused area of the aquifer, the area of attainment (AOA). Contaminated water is treated by solar evaporation at an existing facility at the LM repository.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

Monticello Mill Tailings Site Operable Unit III Annual Groundwater Report May 2014 Through April 2015, October 2015

This report provides the annual analysis of water quality restoration progress, cumulative through April 2015, for Operable Unit (OU) III, surface water and groundwater, of the U.S. Department of Energy (DOE) Office of Legacy Management Monticello Mill Tailings Site (MMTS). The MMTS is a Comprehensive Environmental Response, Compensation, and Liability Act National Priorities List site located in and near the city of Monticello, San Juan County, Utah. MMTS comprises the 110-acre site of a former uranium- and vanadium-ore-processing mill (mill site) and 1,700 acres of surrounding private and municipal property. Milling operations generated 2.5 million cubic yards of waste (tailings) from 1942 to 1960. The tailings were impounded at four locations on the mill site. Inorganic constituents in the tailings drained from the impoundments to contaminate local surface water (Montezuma Creek) and groundwater in the underlying alluvial aquifer. Mill tailings dispersed by wind and water also contaminated properties surrounding and downstream of the mill site. Remedial actions to remove and isolate radiologically contaminated soil, sediment, and debris from the former mill site (OU I) and surrounding properties (OU II) were completed in 1999 with the encapsulation of the wastes in an engineered repository located on DOE property 1 mile south of the former mill site. Contamination of groundwater and surface water remains within OU III at levels that exceed water quality protection standards. Uranium is the primary contaminant of concern. LM implemented monitored natural attenuation with institutional controls as the OU III remedy in 2004. Because groundwater restoration proceeded more slowly than expected and did not meet performance criteria established in the OU III Record of Decision (June 2004), LM implemented a contingency action in 2009 by an Explanation of Significant Difference to include a pump-and-treat system using a single extraction well and treatment by zero-valent iron (ex-situ treatment system). The contingency action was optimized in 2015 with the installation of 8 extraction wells and 16 monitoring wells in a focused area of the aquifer (area of attainment). Contaminated water is treated by solar evaporation at an existing onsite LM facility. Environmental monitoring at OU III consists of twice-yearly (April and October) collection and analysis of hydrologic and water-quality data from an established network of observation wells, seeps, and surface water locations. The scope of monitoring was expanded in 2009 for the ex situ treatment system and in 2015 for the remedy optimization system. Operation and monitoring of the ex situ treatment system was discontinued in 2014 with the start-up of the remedy optimization system. No data anomalies for OU III water quality trending or restoration progress are identified for the May 2014 through April 2015 reporting period. Although some regions of the aquifer demonstrate decreasing concentration trends, such trending is not evident for the bulk of the aquifer and a prolonged restoration period is indicated. The groundwater contingency remedy optimization system captures significant contaminant mass (primarily uranium) from the area of attainment; however, because that system only became operational in 2015, a long-term forecast of restoration progress is premature.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2014

Anomalous grain refinement trends during mechanical milling of Bi 2 Te 3

The structural evolution of nanocrystalline bismuth telluride (Bi 2 Te 3 ) during mechanical milling is investigated here under different milling energies and temperatures. After prolonged milling, the compound evolves toward a steady-state nanostructure that is found to be unusually strongly dependent on the processing conditions. In contrast to most literature on mechanical milling, in Bi 2 Te 3 we find that the smallest steady-state grain sizes are attained under the lowest energy milling conditions. An analysis based on the balance between refinement and recovery in the steady state shows that two regimes of behavior are expected based on the thermo-physical properties of the milled powder. Bi 2 Te 3 lies in a relatively unusual regime where greater impact energy promotes adiabatic heating and recovery more than it does defect accumulation; hence more intense milling leads to larger steady-state grain sizes. Implications for other materials are discussed with reference to a “milling intensity map” that delineates the set of material properties for which this behavior will be observed.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Calorimetric study on mechanically milled aluminum and multiwall carbon nanotube composites

Pure aluminum reinforced with carbon nanotube (CNT) composites have been prepared by high energy attritor milling up to 48 hrs. Differential Scanning Calorimetry (DSC) has been carried out to investigate apparent activation energy and order of the reaction between carbon nanotubes and aluminum by Kissinger equation and Crane equation under non-isothermal conditions. The DSC results clearly reveal that an exothermic reaction occurs before the melting of aluminum. The effect of milling time on the initiation of this exothermic reaction has been studied. The peak temperature of the reaction of carbon nanotubes and aluminum is found to depend on the heating rate during the continuous heating. Apparent activation energy was found to get doubled after milling for 36 hrs compared to 24 hrs milled samples. The mechanism of the reaction kinetics which depends on reaction order is instantaneous nucleation and one dimensional growth for both samples. Formation of Al{sub 4}C{sub 3} was confirmed by X-ray diffraction (XRD) of as-milled powders and after performing DSC of the milled powders. Highlights: {yields} Attritor milling used for processing Al-CNT composites. {yields} Powder morphology as a function of time studied. {yields} Apparent activation energy and order of the reaction calculated for Al{sub 4}C{sub 3} formation. {yields} Apparent activation energy increases two fold with increase in milling time from 24 to 36 hours.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Thermoelectric properties of BiSbTe-type alloys prepared by chill-casting and cryo-milling

The thermoelectric properties of Bi x Sb 1-x Te 3 processed through milling have been extensively studied with varied results that needs to be rationalized. Since cryo-milling is a relatively cleaner milling process compared to other milling processes, in this study we explore this technique to reduce the particle size prior to compaction to get an insight into the thermoelectric properties. We first report the results of cryomilled BiSbTe 3 compacted by spark plasmas sintering (SPS) process and show that milling leads to a change in transport behavior from ‘p’ to ‘n’ type similar to that reported for Bi 2 Te 3 . It is shown that the defects induced by milling is responsible for this change in materials behavior. We further study the effect of change in Bi to Sb ratio and excess tellurium on the thermoelectric properties when processed through cryo-milling as well as casting using a chilled copper block. Excess tellurium leads to a microstructure containing a fraction of layered eutectic that gets further fragmented during cryo-milling. Although the Seebeck coefficient does not change significantly, reflecting the cleanliness of the process, the thermal conductivity changes during hot compaction leading to an improvement of ZT. However, a comparison of all the reported results does not reveal any systematics in thermoelectric properties reflecting the difficulties with these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Microstructural evolution of nanostructured Ti{sub 0.7}Ni{sub 0.3}N prepared by reactive ball-milling

Graphical abstract: - Highlights: • α-Ti to β-Ti phase conversion is observed during 1 h of milling. • Ti{sub 0.7}Ni{sub 0.3}N (fcc) phase is noticed to form after 1 h of milling. • Formation time of Ti(Ni,N) phase is same as TiN phase. • Both X-ray and HRTEM microstructure characterization revealed similar results. - Abstract: Nanocrystalline stoichiometric Ti{sub 0.7}Ni{sub 0.3}N powder has been synthesized by ball-milling the α-Ti (hcp) and Ni (fcc) powders under N{sub 2} gas at room temperature. The α-Ti phase partially transforms to the transient (-Ti phase after 1 h of milling. After 5.5 h of milling, very broad reflections of Ti{sub 0.7}Ni{sub 0.3}N phase is noticed. Complete formation of Ti{sub 0.7}Ni{sub 0.3}N phase is observed after 9 h of milling. Microstructure in terms of lattice imperfections of unmilled and all ball-milled powder mixtures are primarily characterized by analyzing the X-ray powder diffraction patterns employing the Rietveld structure refinement procedure. It clearly reveals the presence of Ti{sub 0.7}Ni{sub 0.3}N phase and inclusion of nitrogen atoms into the α-Ti–Ni matrix on the way to formation of nitride phase. Microstructure of the ball milled nitride powders is also characterized by HRTEM. Particle size of Ti{sub 0.7}Ni{sub 0.3}N phase obtained from XRD method of characterization is ∼5 nm which is very close to that obtained from HRTEM.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Microstructure and martensitic transformation in Si-coated TiNi powders prepared by ball milling

Graphical abstract: - Highlights: • Amorphous Si-coated TiNi powders were prepared successfully by ball milling. • Ti{sub 4}Ni{sub 4}Si{sub 7} was formed at the interface between Si and TiNi after annealing. • Si-coated Ti–Ni powders displayed the R phase after annealing. - Abstract: Si was coated on the surface of Ti–49Ni (at%) alloy powders by ball milling in order to improve the electrochemical properties of the Si electrodes of secondary Li ion batteries and then the microstructure and martensitic transformation behavior were investigated by means of scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Ti–Ni powders coated with Si were fabricated successfully by ball milling. As-milled powders consisted of highly deformed Ti–Ni powders with the B2 phase and amorphous Si layers. The thickness of the Si layer coated on the surface of the Ti–Ni powders increased from 3–5 μm to 10–15 μm by extending the milling time from 3 h to 48 h. However, severe contamination from the grinding media, ZrO{sub 2} occurred when the ball milling time was as long as 48 h. By heating as-milled powders to various temperatures in the range of 673–873 K, the highly deformed Ti–Ni powders were recovered and Ti{sub 4}Ni{sub 4}Si{sub 7} was formed. Two-stage B2–R–B19′ transformation occurred when as-milled Si-coated Ti–49Ni alloy powders were heated to temperatures below 873 K, above this temperature one-stage B2–B19′ transformation occurred.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Mechanism of Ball Milling Effect on Carbothermic Reduction of Industrial Magnesia by Coke

Mechanical milling always improves the chemical reaction rate in the metallurgy process. The experiment proved that ball milling treatment on raw materials, including industrial magnesia, metallurgical coke, and fluoride calcium, could increase greatly the reaction rate of magnesia. The reaction samples and residues were analyzed by particle size measurement, X-ray diffraction (XRD) analysis, Raman spectroscopy analysis, scanning electron microscope (SEM), and transmission electron microscope (TEM). The results suggested that the positive effect of ball milling on the reaction rate came from three aspects. Ball milling could decrease magnesia particle size and peel coke into graphite sheets to enlarge their contact surface. Meanwhile, ball milling could slightly destroy the crystal grain surface of magnesia and decrease the crystallization of graphite. The nanometer-scale magnesia particles and graphite sheets would stably and strongly attract together after a longer time ball milling. The possible evolution of the particles during ball milling was given, which explained the mechanism of the ball milling effect on the carbothermic reduction of industrial magnesia by coke.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Glancing-incidence focussed ion beam milling: A coherent X-ray diffraction study of 3D nano-scale lattice strains and crystal defects

Here, this study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strains have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of Burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗