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At least 91 records · Page 5

Comprehensive characterization of ball-milled powders simulating a tribofilm system

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.

36 MATERIALS SCIENCE↗

Surface integrity and fatigue behaviour of electric discharged machined and milled austenitic stainless steel

Machining of austenitic stainless steels can result in different surface integrities and different machining process parameters will have a great impact on the component fatigue life. Understanding how machining processes affect the cyclic behaviour and microstructure are of outmost importance in order to improve existing and new life estimation models. Milling and electrical discharge machining (EDM) have been used to manufacture rectangular four-point bend fatigue test samples; subjected to high cycle fatigue. Before fatigue testing, surface integrity characterisation of the two surface conditions was conducted using scanning electron microscopy, surface roughness, residual stress profiles, and hardness profiles. Differences in cyclic behaviour were observed between the two surface conditions by the fatigue testing. The milled samples exhibited a fatigue limit. EDM samples did not show the same behaviour due to ratcheting. Recrystallized nano sized grains were identified at the severely plastically deformed surface of the milled samples. Large amounts of bent mechanical twins were observed ~ 5 μm below the surface. Grain shearing and subsequent grain rotation from milling bent the mechanical twins. EDM samples showed much less plastic deformation at the surface. Surface tensile residual stresses of ~ 500 MPa and ~ 200 MPa for the milled and EDM samples respectively were measured. - Highlights: •Milled samples exhibit fatigue behaviour, but not EDM samples. •Four-point bending is not suitable for materials exhibiting pronounced ratcheting. •LAGB density can be used to quantitatively measure plastic deformation. •Grain shearing and rotation result in bent mechanical twins. •Nano sized grains evolve due to the heat of the operation.

36 MATERIALS SCIENCE↗

Effect of ball milling conditions on microstructure and lithium storage properties of LiNi0.5Mn1.5O4 as cathode for lithium-ion batteries

Highlights: • Precursors of LNM respectively synthesized by dry and wet ball-milling. • Under wet ball-milling raw materials form slurry and mix well in microscale. • LNM-w12 sample presents proper stoichiometric composition and the highest D{sub Li}{sup +}. • At 0.1 C rate LNM-w12 delivers 133 mAh g{sup −1} at 100 cycle close to theoretical value. • LNM-w12 delivers 97 mAh g{sup −1} at 10 C rate and remains 78% after 1000 cycles. - Abstract: In this work, the precursors of LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} (LNM) are respectively synthesized by dry and wet ball-milling. Under wet ball-milling, the problem of sticky residue in dry ball-milling is effectively resolved, the three raw materials form homogeneous slurry and mix well in micrometers level. LNM-w12 sample synthesized by using precursor added 12 mL milling medium gains the atomic composition closed to the theoretical value, ordered crystal structure and the highest lithium diffusion coefficient. At 0.1 C rate, LNM-w12 delivers the capacity of 136 mAh g{sup −1} at the first cycle, and 133 mAh g{sup −1} at the 100th cycle. Moreover, LNM-w12 delivers the initial capacity of 97 mAh g{sup −1} at 10 C rate, and remains 78% after 1000 cycles. The great rate capability of LNM-w12 can be attributed to the well-formed crystal structure, ordered and stable surface structure, which is conducive to the diffusion of lithium ions and prevents the dissolution of the material at high voltage.

25 ENERGY STORAGE↗

Synthesis of a Mg-based alloy with a hydrogen-storage capacity of over 7 wt% by adding a polymer CMC via transformation-involving milling

Highlights: • Preparation of a polymer Carboxymethylcellulose (CMC)-added Mg alloy by milling in hydrogen. • Hydrogen-storage capacity of about 7.2 wt% by activated Mg-5CMC at 593 K in hydrogen of 12 bar. • A very high initial hydrogen uptake rate of 1.45 wt% H/min at 593 K in 12 bar hydrogen after activation. • Addition of CMC is more effective than additions of halogen compounds, oxides, or metals. • First study where CMC is added by milling in hydrogen to improve hydrogen-storage properties of Mg. - Abstract: Carboxymethylcellulose sodium salt (CMC) was added to magnesium via milling in hydrogen (transformation-involving milling), and samples with compositions of 95 wt% Mg + 5 wt% CMC (named Mg-5CMC) and 90 wt% Mg + 10 wt% CMC (Mg-10CMC) were prepared. At the cycle number (CN) of three, Mg-5CMC had a very high initial hydrogenation rate (1.45 wt% H/min) and a very large effective hydrogen-storage capacity of about 7.2 wt%. It is believed that the CMC melted during milling, and that because the melted CMC was highly viscous, sliding between the Mg particles and hardened steel balls was prevented, which led to effective milling (the generation of defects and cracks and the reduction of particle sizes). To the best of our knowledge, this study is the first in which a polymer CMC was added to Mg in order to improve the hydrogenation and dehydrogenation properties of Mg.

36 MATERIALS SCIENCE↗

Determination of Specific Forces and Tool Deflections in Micro-milling of Ti-6Al-4V alloy using Finite Element Simulations and Analysis

Titanium alloys offer superb properties in strength, corrosion resistance and biocompatibility and are commonly utilized in medical devices and implants. Micro-end milling process is a direct and rapid fabrication method for manufacturing medical devices and implants in titanium alloys. Process performance and quality depend upon an understanding of the relationship between cutting parameters and forces and resultant tool deflections to avoid tool breakage. For this purpose, FE simulations of chip formation during micro-end milling of Ti-6Al-4V alloy with an ultra-fine grain solid carbide two-flute micro-end mill are investigated using DEFORM software.At first, specific forces in tangential and radial directions of cutting during micro-end milling for varying feed advance and rotational speeds have been determined using designed FE simulations for chip formation process. Later, these forces are applied to the micro-end mill geometry along the axial depth of cut in 3D analysis of ABAQUS. Consequently, 3D distributions for tool deflections and von Misses stress are determined. These analyses will yield in establishing integrated multi-physics process models for high performance micro-end milling and a leap-forward to process improvements.

36 MATERIALS SCIENCE↗

New findings on the atomistic mechanisms active during mechanical milling of a Fe-Y{sub 2}O{sub 3} model alloy

In order to improve the mechanical properties at elevated temperatures, several types of steels are mechanically alloyed with yttria. The processes that are active during milling differ dependent on the individual powder constituents. Nevertheless, some theories exist which try to describe the mechanism of producing a metastable phase during milling. However, even in the system iron–yttria, the mechanisms taking place during milling are still not well understood. By using the example of a simple iron–yttria model alloy, this paper attempts to elucidate the structure of mechanically milled powder particles and, consequently, to clarify the functionality of mechanical alloying in the last stage of milling. Positron annihilation experiments on milled materials revealed “open” volumes which are enriched in yttria. Electron backscatter diffraction and atom probe tomography as complimentary techniques allowed an identification of these “open” volumes as mainly vacancies, where enrichments of Y and O occur. From these results, it can be concluded that especially vacancies are responsible for producing a metastable phase, whereby yttria is dissolved in pure iron.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of Composition on the Phase Structure and Magnetic Properties of Ball-Milled LaFe11.71-xMnxSi1.29H1.6 Magnetocaloric Powders

Magnetocaloric alloys are an important class of materials that enable non-vapor compression cycles. One promising candidate for magnetocaloric systems is LaFeMnSi, thanks to a combination of factors including low-cost constituents and a useful curie temperature, although control of the constituents’ phase distribution can be challenging. In this paper, the effects of composition and high energy ball milling on the particle morphology and phase stability of LaFe11.71-xMnxSi1.29H1.6 magnetocaloric powders were investigated. The powders were characterized with optical microscopy, dynamic light scattering, X-ray diffraction (XRD), and differential scanning calorimetry (DSC). It was found that the powders retained most of their original magnetocaloric phase during milling, although milling reduced the degree of crystallinity in the powder. Furthermore, some oxide phases (<1 weight percent) were present in the as-received and milled powders, which indicates that no significant contamination of the powders occurred during milling. Finally, the results indicated that the Curie temperature drops as Fe content decreases (Mn content increases). In all of the powders, milling led to an increase in the Curie temperature of ~3–6 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Control of Y₂O₃ phase and its nanostructure formation through a very high energy mechanical milling

The formation behavior of Y₂O₃ ceramic particles was studied by employing a very high energy ball milling (milling energy: ~165 kJ/g·hit, milling speed: 1000 rpm). Both the XRD and HRTEM studies revealed that the high impact strain energy generated during the milling caused a drastic phase transition from the original C-type cubic (space group Ia3, a=10.58 Å) to the metastable B-type monoclinic (space group C2/m, a=13.89 Å), finally followed by a partial solid-state amorphization. The cubic phase was difficult to be reduced down to smaller than 10 nm, while the monoclinic phase was stabilized at sizes smaller than 10 nm with a mean crystallite size of 7.57 nm. Consequently, the existence of Y₂O₃ at a nanoscale smaller than 10 nm is possible by forming metastable monoclinic crystals, which are strain-induced. - Graphical abstract: The fig shows the solid-state phase formation of Y₂O₃ by very high energy input into the particles during milling: ordered body-centered cubic phase (space group Ia3, a=10.58 Å) nanocrystalline monoclinic phase (space group C2/m, a=13.89 Å) disordered monoclinic phase partial amorphous phase. The formation of Y₂O₃ smaller than 10 nm was strongly dependent on whether the phase transition from cubic to monoclinic occurred. Highlights: • This paper analyses very high energy milling behavior of coarse Y₂O₃ particles. • A drastic phase transition from cubic to monoclinic occurred with a partial amorphization. • An existence of Y₂O₃ smaller than 10 nm is possible by forming strain-induced monoclinic crystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Study of morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled compound

The morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled intermetallic compounds are presented. The polycrystalline HoNi{sub 3} bulk compound crystallizes in the rhombohedral PuNi{sub 3} — type of crystal structure and indicates ferrimagnetic arrangement with the Curie temperature of T{sub C} = 57 ± 2 K, the helimagnetic temperature T{sub h} = 23 ± 2 K with the total saturation magnetic moment of 6.84 μ{sub B}/f.u. at 2 K. The use of the ball-milling method leads to the formation of HoNi{sub 3} nanoflakes with typical thickness of less than 100 nm prone to agglomeration upon milling. The increase of grinding duration leads to the reduction in crystallite size, which was confirmed by various complementary microscopical and diffraction studies. Moreover, the increase in milling duration results in the emergence of the relatively small coercivity (H{sub C}), remanence (M{sub r}) and a variation of the saturation magnetization (M{sub S}). - Graphical abstract: Display Omitted - Highlights: • The ball-milling method exhibits significant potential for producing RT{sub 3} nanopowders. • The AFM method was used for the first time in analysis of R–T nanoflakes morphology. • HoNi{sub 3} compound forms polycrystalline and textured nanoflakes evolving upon milling. • The decrease in crystallite size via grinding is confirmed by XRD, TEM and AFM. • The magnetic parameters were sensitive to the extension of pulverization b.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The effect of ball-milling time and annealing temperature on fracture toughness of Ni-3 wt.% SiC using small punch testing

Highlights: • The fracture energy of Ni-SiC is strongly dependent on the grain size of Ni matrix • The ball-milling time governs the fracture behaviour of Ni-3 wt.% SiC • A higher proportion of big SiC particles at grain boundary is responsible for a lower fracture toughness - Abstract: A set of dispersion strengthened Ni-3 wt.% SiC samples have been prepared via a powder metallurgy route for an application in molten salt reactor (MSR) systems. A mixture of 97 wt.% Ni and 3 wt.% SiC powder was prepared by varying the ball-milling time (8, 24, 36 and 48 h). The ball-milling process was followed by powder consolidation using spark plasma sintering (SPS) and rapid cooling to room temperature. The samples were then annealed at different temperatures (300 °C, 700 °C and 850 °C). The fracture behaviour of the Ni-3 wt.% SiC samples was investigated using the Small Punch Test (SPT). A scanning electron microscope (SEM) with energy dispersive spectrometer (EDS) and electron back-scatter diffraction (EBSD), as well as transmission electron microscopy (TEM) were employed to examine the microstructure of the tested Ni-3 wt.% SiC samples. The obtained results show that the SPT fracture energy is strongly dependent on the grain size of Ni matrix, which is affected by ball-milling times and annealing temperature. It has been further found that the segregation of large SiC particles at grain boundaries promotes intergranular fracture and thus significantly reduces the fracture energy. The results indicate that the distribution and size of SiC particles at grain boundary is mainly affected by the ball-milling time. Hence, the ball-milling time governs the fracture toughness of Ni-3 wt.% SiC samples.

36 MATERIALS SCIENCE↗

Factors influencing the ball milling of Si3N4 in water

A statistical study of the ball milling of Si3N4 powder in Si3N4 hardware was undertaken to understand how the resulting increase in specific surface area is related to solids loading and mill speed. An attempt was made to optimize milling conditions. The degree of communication was more dependent upon solids loading than mill speed. A practical grinding limit between 0.5 and 0.75 microns was achieved in 144 hr independent of solids loading. Ball mill wear and media wear were independent of both solids loading and mill speed.

Freedman, M. R.↗

Project Independence: Construction of an Integrated Biorefinery for Production of Renewable Biofuels at an Existing Pulp and Paper Mill

Project Independence proposed to construct a demonstration biomass-to-liquids (BTL) biorefinery in Wisconsin Rapids, isconsin. The biorefinery was to be co-located at the existing pulp and paper mill, NewPage Wisconsin System Incorporated’s Wisconsin Rapids Mill, and when in full operation would both generate renewable energy for Wisconsin Rapids Mill and produce liquid fuels from abundant and renewable lignocellulosic biomass. The biorefinery would serve to validate the thermochemical pathway and economic models for BTL production using forest residuals and wood waste, providing a basis for proliferating BTL conversion technologies throughout the United States. It was a project goal to create a compelling new business model for the pulp and paper industry, and support the nation’s goal for increasing renewable fuels production and reducing its dependence on foreign oil. NewPage Corporation planned to replicate this facility at other NewPage Corporation mills after this first demonstration scale plant was operational and had proven technical and economic feasibility. An overview of the process begins with biomass being harvested, sized, conditioned and fed into a ThermoChem Recovery International (TRI) steam reformer where it is converted to high quality synthetic gas (syngas). The syngas is then cleaned, compressed, scrubbed, polished and fed into the Fischer-Tropsch (F-T) catalytic reactors where the gas is converted into two, sulfur-free, clean crude products which will be marketed as revenue generating streams. Additionally, the Fischer-Tropsch products could be upgraded for use in automotive, aviation and chemical industries as valuable products, if desired. As the Project Independence project set out to prove forest products could be used to commercially produce biofuels, they planned to address and mitigate issues as they arose. In the early days of the Project Independence project, the plant was sized to process 500 dry tons of biomass per day but would generate a blend of synthesis gas for the lime kiln and a minimum of Fischer-Tropsch liquids for sale. This was to be done using a single stage of Fischer-Tropsch reaction at roughly a 70% yield. The capability of the Wisconsin Rapids Mill lime kiln to run on the relatively low heating value of the product synthesis gas was problematic. The design was then changed to maximize Fischer-Tropsch liquids production using a two stage Fischer-Tropsch process. Project Independence progressed with the design of the mill as ThermoChem Recovery International worked on the technical details of the project as well as develop information from their pilot plant. The pilot plant work uncovered several problems with the synthesis gas clean-up that solutions. ThermoChem Recovery International found these solutions and developed a very good path forward on the technical side. The technical solutions were demonstrated in the pilot plant to everyone’s satisfaction. In July 2010, NewPage Corporation had been severely affected by the downturn in the economy and actively went to find a strategic partner. By April 2011 the Abell Foundation entered the picture as this strategic partner. The Abell Foundation would join forces as Project Independence Inc. to build the 500 dry ton per day Project Independence plant. The design of this facility progress even after NewPage Corporation declared Chapter 11 Bankruptcy protection in September, 2011. This continued until April 2012 when NewPage Corporation determined that continued work on Project Independence Inc. presented too much risk with little reward for NewPage Corporation. The project was terminated at this point.

09 BIOMASS FUELS↗

Life-Cycle Greenhouse Gas Emission Impacts of Forest Residue Pre-processing with Wet Milling

The goal of this analysis was to evaluate the environmental impact of a Case Study that uses wet milling to preprocess logging residues before feeding to a catalytic fast pyrolysis conversion step. The results of the Case Study were compared to those of the status quo Base Case system where dry milling is used. The results reveal that wet milling achieved 65% lower GHG emissions per dry ton of conversion-ready feedstock than the conventional dry milling technology. This is mainly because wet milling greatly reduced the energy consumption for drying. In addition, wet milling also generates fewer fines, thus improving the throughput of conversion-ready feedstock

biomass preprocessing↗

Overview of the Long-Term Stewardship of the Remediated Uranium Mining and Milling Sites in Europe - 20079

Uranium mining in Europe began in the ' 40's for civil and military applications. The great majority of the uranium mines have now been closed and are going through the stages of decommissioning and/or rehabilitation. Today, the main uranium producers are outside the EU; only a few mines are still in operation inside the EU. In 2006, the situation of the uranium mines and mill tailings in Europe, identifying the tailings liabilities, their status, the plans for these sites and any associated hazards, was reported to the EC. The legacy of uranium mines and mill tailing disposals in the EU are located mainly in 12 Member States where, in total, 87 tailing objects were identified at 63 sites. The volume of each one of these tailings disposal varies from a few thousand to several tens of million m{sup 3}. The majority of these sites are no longer in operation. More than 40 tailing embankments have already been completely remediated. Approximately 20 are currently being remediated while for the remaining objects, remediation has yet to start. After ten years, and for a few cases where the respective projects have not yet been completed, it seems that most of Europe's uranium mines and milling legacies were remediated according to acceptable environmental standards. Nevertheless, Europe is about to face a new challenge that comes from the concluded remediation projects for which an effective set of measures for coordinated institutional control, known as 'long-term stewardship', is needed including, in most cases, continuous and active maintenance. Moreover, the uncertainty of what will happen to these sites if institutional control fails at some point in time is a major concern. This work presents a summary of the situation and current issues of the uranium mine and mill tailings in Europe and their remediation status. It addresses not only the management of existing uranium mine and mill legacies but also the methods and strategies that have been used to prevent the creation of new future legacy sites from uranium mines still in operation. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Production of Rounded Reactive Composite Ti/Al Powders for Selective Laser Melting by High-Energy Ball Milling

The effect of different regimes of high-energy ball milling (HEBM) on the morphology of reactive Ti–Al powders was studied. It is shown that a “soft” regime of mechanical treatment can be readily used to prepare spheroidal reactive Ti–Al powders with the flow ability suitable for selective laser melting applications. Size distribution of milled powders was found to depend on the diameter of milling balls. Milled powders showed good flow ability of 61.7 and 81.25 s for 2-mm and 6-mm balls, respectively. Combustion reaction in the compacts prepared from milled powders got started at temperatures close to the melting point of Al, and due to the thermal effect of reaction, the temperature jump made a value of about 500°C. The combustion product—Ti–TiAl{sub 3} composite—can be recommended for use as a high-temperature structural material.

36 MATERIALS SCIENCE↗

Development of Fe-9Cr Alloy via High-Energy Ball Milling and Spark Plasma Sintering

Iron and chromium powders were mixed and mechanically alloyed via high-energy ball milling for different time durations (2–20 h) to produce an alloy powder with a nominal composition of Fe-9Cr (wt.%). The milled Fe-9Cr powders were analyzed using scanning electron microscopy (SEM), x-ray diffraction (XRD) and transmission electron microscopy (TEM) to understand the impact of ball milling (BM) time on the characteristics of the milled powder. The optimized milled powder samples were then consolidated via spark plasma sintering (SPS) for different dwell times and temperatures. The density of consolidated samples was found to reach a maximum of 98%. Microstructural characterization of the SPS samples were performed using XRD, SEM, TEM and electron backscatter diffraction. This study highlights the principles and importance of high-energy BM and SPS of Fe-9Cr model alloy for the future development of more complex oxide dispersion-strengthened alloys for various applications including advanced nuclear reactor applications.

36 MATERIALS SCIENCE↗

Mechanics and energetics modeling of ball-milled metal foil and particle structures

The reported research establishes a semi-analytical computational predictive model of fractal microstructure in ball-milled metal foils and powder particulates, with emphasis on its transformation mechanics via an energy-based approach. The evolving structure is composed of reconfigurable warped ellipsoid material domains, subjected to collisions with the ball milling impactors following Brownian motion energetics. In the first step of the model, impacts are assumed to generate ideal Hertzian elastic stress fields, with associated bulk deformations quantified as per Castigliano's strain energy methods. In the second stage of the model, elastic energies are recast to produce frictional slip and plastic yield, thus resulting in surface micro-joints. Only two parameters of the model necessitate experimental calibration, performed by comparison of joint energy with laboratory tensile measurements on ball-milled multilayer Al-Ni foils. Model predictions of evolving internal microstructure are validated against SEM micrographs of Al-Ni powder particulate samples for different ball milling durations. Results demonstrate the capability of the model to accurately capture relevant fractal measures of the microstructure of ball-milled powders.

36 MATERIALS SCIENCE↗

Grinding energy and physical properties of chopped and hammer-milled barley, wheat, oat, and canola straws

In the present study, specific energy for grinding and physical properties of wheat, canola, oat and barley straw grinds were investigated. The initial moisture content of the straw was about 0.13–0.15 (fraction total mass basis). Particle size reduction experiments were conducted in two stages: (1) a chopper without a screen, and (2) a hammer mill using three screen sizes (19.05, 25.4, and 31.75 mm). The lowest grinding energy (1.96 and 2.91 kWh t-1) was recorded for canola straw using a chopper and hammer mill with 19.05-mm screen size, whereas the highest (3.15 and 8.05 kWh t-1) was recorded for barley and oat straws. The physical properties (geometric mean particle diameter, bulk, tapped and particle density, and porosity) of the chopped and hammer-milled wheat, barley, canola, and oat straw grinds measured were in the range of 0.98–4.22 mm, 36–80 kg m-3, 49–119 kg m-3, 600–1220 kg m-3, and 0.9–0.96, respectively. The average mean particle diameter was highest for the chopped wheat straw (4.22-mm) and lowest for the canola grind (0.98-mm). The canola grinds produced using the hammer mill (19.05-mm screen size) had the highest bulk and tapped density of about 80 and 119 kg m-3; whereas, the wheat and oat grinds had the lowest of about 58 and 88–90 kg m-3. The results indicate that the bulk and tapped densities are inversely proportional to the particle size of the grinds. The flow properties of the grinds calculated are better for chopped straws compared to hammer milled using smaller screen size (19.05 mm).

09 BIOMASS FUELS↗