The use of inverse phase gas chromatography to measure the surface energy of crystalline, amorphous, and recently milled lactose.

PubMed

Newell, H E; Buckton, G; Butler, D A; Thielmann, F; Williams, D R

2001-05-01

To assess differences in surface energy due to processing induced disorder and to understand whether the disorder dominated the surfaces of particles. Inverse gas chromatography was used to compare the surface energies of crystalline, amorphous, and ball milled lactose. The milling process made ca 1% of the lactose amorphous, however the dispersive contribution to surface energy was 31.2, 37.1, and 41.6 mJ m(-2) for crystalline, spray dried and milled lactose, respectively. A physical mixture of crystalline (99%) and amorphous (1%) material had a dispersive surface energy of 31.5 mJ m(-2). Milling had made the surface energy similar to that of the amorphous material in a manner that was very different to a physical mixture of the same amorphous content. The milled material will have similar interfacial interactions to the 100% amorphous material.

Powder properties of hydrogenated ball-milled graphite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Y., E-mail: y.zhang062012@gmail.com; Wedderburn, J.; Harris, R.

2014-12-15

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 tomore » 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.« less

Kinetic parameters of grinding media in ball mills with various liner design and mill speed based on DEM modeling

NASA Astrophysics Data System (ADS)

Khakhalev, P. A.; Bogdanov, VS; Kovshechenko, V. M.

2018-03-01

The article presents analysis of the experiments in the ball mill of 0.5x0.3 m with four different liner types based on DEM modeling. The numerical experiment always complements laboratory research and allow obtaining high accuracy output data. An important property of the numerical experiment is the possibility of visualization of the results. The EDEM software allows calculating trajectory of the grinding bodies and kinetic parameters of each ball for the relative mill speed and the different types of mill’s liners.

Solid state amorphization kinetic of alpha lactose upon mechanical milling.

PubMed

Caron, Vincent; Willart, Jean-François; Lefort, Ronan; Derollez, Patrick; Danède, Florence; Descamps, Marc

2011-11-29

It has been previously reported that α-lactose could be totally amorphized by ball milling. In this paper we report a detailed investigation of the structural and microstructural changes by which this solid state amorphization takes place. The investigations have been performed by Powder X-ray Diffraction, Solid State Nuclear Magnetic Resonance ((13)C CP-MAS) and Differential Scanning Calorimetry. The results reveal the structural complexity of the material in the course of its amorphization so that it cannot be considered as a simple mixture made of a decreasing crystalline fraction and an increasing amorphous fraction. Heating this complexity can give rise to a fully nano-crystalline material. The results also show that chemical degradations upon heating are strongly connected to the melting process. Copyright © 2011 Elsevier Ltd. All rights reserved.

A new approach for remediation of As-contaminated soil: ball mill-based technique.

PubMed

Shin, Yeon-Jun; Park, Sang-Min; Yoo, Jong-Chan; Jeon, Chil-Sung; Lee, Seung-Woo; Baek, Kitae

2016-02-01

In this study, a physical ball mill process instead of chemical extraction using toxic chemical agents was applied to remove arsenic (As) from contaminated soil. A statistical analysis was carried out to establish the optimal conditions for ball mill processing. As a result of the statistical analysis, approximately 70% of As was removed from the soil at the following conditions: 5 min, 1.0 cm, 10 rpm, and 5% of operating time, media size, rotational velocity, and soil loading conditions, respectively. A significant amount of As remained in the grinded fine soil after ball mill processing while more than 90% of soil has the original properties to be reused or recycled. As a result, the ball mill process could remove the metals bound strongly to the surface of soil by the surface grinding, which could be applied as a pretreatment before application of chemical extraction to reduce the load.

Structural and Kinetic Hydrogen Sorption Properties of Zr0.8Ti0.2Co Alloy Prepared by Ball Milling

PubMed Central

He, Hui; Tang, Tao; Huang, Zhiyong; Sang, Ge; Zhang, Guanghui; Ba, Jingwen; Liu, Meng

2018-01-01

The effects of ball milling on the hydrogen sorption kinetics and microstructure of Zr0.8Ti0.2Co have been systematically studied. Kinetic measurements show that the hydrogenation rate and amount of Zr0.8Ti0.2Co decrease with increasing the ball milling time. However, the dehydrogenation rate accelerates as the ball milling time increases. Meanwhile, the disproportionation of Zr0.8Ti0.2Co speeds up after ball milling and the disproportionation kinetics is clearly inclined to be linear with time at 500°C. It is found from X-ray powder diffraction (XRD) results that the lattice parameter of Zr0.8Ti0.2Co gradually decreases from 3.164 Å to 3.153 Å when the ball milling time extends from 0 h to 8 h, which is mainly responsible for the hydrogen absorption/desorption behaviors. In addition, scanning electron microscope (SEM) images demonstrate that the morphology of Zr0.8Ti0.2Co has obviously changed after ball milling, which is closely related to the hydrogen absorption kinetics. Besides, high-resolution transmission electron microscopy (HRTEM) images show that a large number of disordered microstructures including amorphous regions and defects exist after ball milling, which also play an important role in hydrogen sorption performances. This work will provide some insights into the principles of how to further improve the hydrogen sorption kinetics and disproportionation property of Zr0.8Ti0.2Co. PMID:29721128

DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, AND ORE BIN CHUTE, LOOKING EAST NORTHEAST. CRUSHED ORE FROM THE SECONDARY ORE BIN WAS INTRODUCED INTO THE FEED TROUGH VIA A CHUTE. AS THE BALL MILL TURNED, THE ROUND SCOOP ALSO TURNED IN THE TROUGH TO CHANNEL ORE INTO THE BALL MILL. SEE CA-292-14 FOR IDENTICAL B&W NEGATIVE. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, AND ORE BIN CHUTE, LOOKING EAST NORTHEAST. CRUSHED ORE FROM THE SECONDARY ORE BIN WAS INTRODUCED INTO THE FEED TROUGH VIA A CHUTE. AS THE BALL MILL TURNED, THE ROUND SCOOP ALSO TURNED IN THE TROUGH TO CHANNEL ORE INTO THE BALL MILL. SEE CA-292-20 (CT) FOR IDENTICAL COLOR TRANSPARENCY. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

Fluid mechanics of slurry flow through the grinding media in ball mills

DOE Office of Scientific and Technical Information (OSTI.GOV)

Songfack, P.K.; Rajamani, R.K.

1995-12-31

The slurry transport within the ball mill greatly influences the mill holdup, residence time, breakage rate, and hence the power draw and the particle size distribution of the mill product. However, residence-time distribution and holdup in industrial mills could not be predicted a priori. Indeed, it is impossible to determine the slurry loading in continuously operating mills by direct measurement, especially in industrial mills. In this paper, the slurry transport problem is solved using the principles of fluid mechanics. First, the motion of the ball charge and its expansion are predicted by a technique called discrete element method. Then themore » slurry flow through the porous ball charge is tackled with a fluid-flow technique called the marker and cell method. This may be the only numerical technique capable of tracking the slurry free surface as it fluctuates with the motion of the ball charge. The result is a prediction of the slurry profile in both the radial and axial directions. Hence, it leads to the detailed description of slurry mass and ball charge within the mill. The model predictions are verified with pilot-scale experimental work. This novel approach based on the physics of fluid flow is devoid of any empiricism. It is shown that the holdup of industrial mills at a given feed percent solids can be predicted successfully.« less

Attempted - to -Phase Conversion of Croconic Acid via Ball Milling

DTIC Science & Technology

2017-05-18

extended milling times may degrade the material. 15. SUBJECT TERMS ball milling, croconic acid, Hertzian stress , C5H2O5, extended solid 16. SECURITY...the motion of the Wig-L-Bug ball mill; from this motion it was possible to determine the velocity parameters needed for Hertzian stress ...Milling Pressures The high pressures achievable in this type of mill result from stresses that develop in the milled material as it is trapped between

Determination of the boundary conditions of the grinding load in ball mills

NASA Astrophysics Data System (ADS)

Sharapov, Rashid R.

2018-02-01

The prospects of application in ball mills for grinding cement clinker with inclined partitions are shown. It is noted that ball mills with inclined partitions are more effective. An algorithm is proposed for calculating the power consumed by a ball mill with inclined inter-chamber partitions in which an axial movement of the ball load takes place. The boundary conditions in which the ball load is located are determined. The equations of bounding the grinding load are determined. The behavior of a grinding load is considered in view of the characteristic cross sections. The coordinates of the centers of gravity of the grinding load with a definite step and the shape of the cross sections are determined. It is theoretically shown that grinding load in some parts of the ball mill not only consumes, but also helps to rotate the ball mill. Methods for calculating complex analytical expressions for determining the coordinates of the centers of gravity of the grinding load under the conditions of its longitudinal motion have developed. The carried out researches allow to approach from the general positions to research of behavior of a grinding load in the ball mills equipped with various in-mill devices.

Micro structrual characterization and analysis of ball milled silicon carbide

NASA Astrophysics Data System (ADS)

Madhusudan, B. M.; Raju, H. P.; Ghanaraja., S.

2018-04-01

Mechanical alloying has been one of the prominent methods of powder synthesis technique in solid state involving cyclic deformation, cold welding and fracturing of powder particles. Powder particles in this method are subjected to greater mechanical deformation due to the impact of ball-powder-ball and ball-powder-container collisions that occurs during mechanical alloying. Strain hardening and fracture of particles decreases the size of the particles and creates new surfaces. The objective of this Present work is to use ball milling of SiC powder for different duration of 5, 10, 15 and 20 hours by High energy planetary ball milling machine and to evaluate the effect of ball milling on SiC powder. Micro structural Studies using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and EDAX has been investigated.

Effect of amorphous Mg{sub 50}Ni{sub 50} on hydriding and dehydriding behavior of Mg{sub 2}Ni alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guzman, D., E-mail: danny.guzman@uda.cl; Ordonez, S.; Fernandez, J.F.

Composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50} was prepared by mechanical milling starting with nanocrystalline Mg{sub 2}Ni and amorphous Mg{sub 50}Ni{sub 50} powders, by using a SPEX 8000 D mill. The morphological and microstructural characterization of the powders was performed via scanning electron microscopy and X-ray diffraction. The hydriding characterization of the composite was performed via a solid gas reaction method in a Sievert's-type apparatus at 363 K under an initial hydrogen pressure of 2 MPa. The dehydriding behavior was studied by differential thermogravimetry. On the basis of the results, it is possible to conclude that amorphous Mg{submore » 50}Ni{sub 50} improved the hydriding and dehydriding kinetics of Mg{sub 2}Ni alloy upon cycling. A tentative rationalization of experimental observations is proposed. - Research Highlights: {yields} First study of the hydriding behavior of composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50}. {yields} Microstructural characterization of composite material using XRD and SEM was obtained. {yields} An improved effect of Mg{sub 50}Ni{sub 50} on the Mg{sub 2}Ni hydriding behavior was verified. {yields} The apparent activation energy for the hydrogen desorption of composite was obtained.« less

Response to Thermal Exposure of Ball-Milled Aluminum-Borax Powder Blends

NASA Astrophysics Data System (ADS)

Birol, Yucel

2013-04-01

Aluminum-borax powder mixtures were ball milled and heated above 873 K (600 °C) to produce Al-B master alloys. Ball-milled powder blends reveal interpenetrating layers of deformed aluminum and borax grains that are increasingly refined with increasing milling time. Thermal exposure of the ball-milled powder blends facilitates a series of thermite reactions between these layers. Borax, dehydrated during heating, is reduced by Al, and B thus generated reacts with excess Al to produce AlB2 particles dispersed across the aluminum grains starting at 873 K (600 °C). AlB2 particles start to form along the interface of the aluminum and borax layers. Once nucleated, these particles grow readily to become hexagonal-shaped crystals that traverse the aluminum grains with increasing temperatures as evidenced by the increase in the size as well as in the number of the AlB2 particles. Ball milling for 1 hour suffices to achieve a thermite reaction between borax and aluminum. Ball milling further does not impact the response of the powder blend to thermal exposure. The nucleation-reaction sites are multiplied, however, with increasing milling time and thus insure a higher number of smaller AlB2 particles. The size of the AlB2 platelets may be adjusted with the ball milling time.

Impact Ignition and Combustion Behavior of Amorphous Metal-Based Reactive Composites

NASA Astrophysics Data System (ADS)

Mason, Benjamin; Groven, Lori; Son, Steven

2013-06-01

Recently published molecular dynamic simulations have shown that metal-based reactive powder composites consisting of at least one amorphous component could lead to improved reaction performance due to amorphous materials having a zero heat of fusion, in addition to having high energy densities and potential uses such as structural energetic materials and enhanced blast materials. In order to investigate the feasibility of these systems, thermochemical equilibrium calculations were performed on various amorphous metal/metalloid based reactive systems with an emphasis on commercially available or easily manufactured amorphous metals, such as Zr and Ti based amorphous alloys in combination with carbon, boron, and aluminum. Based on the calculations and material availability material combinations were chosen. Initial materials were either mixed via a Resodyn mixer or mechanically activated using high energy ball milling where the microstructure of the milled material was characterized using x-ray diffraction, optical microscopy and scanning electron microscopy. The mechanical impact response and combustion behavior of select reactive systems was characterized using the Asay shear impact experiment where impact ignition thresholds, ignition delays, combustion velocities, and temperatures were quantified, and reported. Funding from the Defense Threat Reduction Agency (DTRA), Grant Number HDTRA1-10-1-0119. Counter-WMD basic research program, Dr. Suhithi M. Peiris, program director is gratefully acknowledged.

Effect of milling time on microstructure and properties of Nano-titanium polymer by high-energy ball milling

NASA Astrophysics Data System (ADS)

Wang, Bo; Wei, Shicheng; Wang, Yujiang; Liang, Yi; Guo, Lei; Xue, Junfeng; Pan, Fusheng; Tang, Aitao; Chen, Xianhua; Xu, Binshi

2018-03-01

Nano-titanium (Nano-Ti) was prepared by high-energy ball milling from pure Ti power and grinding agents (Epoxy resin) at room temperature. The effect of milling time on structure and properties of Nano-Ti polymer were investigated systematically. The results show that high-energy ball milling is an effective way to produce Nano-Ti polymer. The dispersion stability and compatibility between Ti power and grinding agents are improved by prolonging the milling time at a certain degree, that is to say, the optimization milling time is 240 min. The particle size of Ti powder and the diffraction peaks intensity of Ti decrease obviously as the milling time increases due to the compression stress, shear friction and other mechanical forces are formed during ball milling. FT-IR result displays that the wavenumber of all the bands move to lower wavenumber after ball milling, and the epoxy ring is open. The system internal energy rises owing to the broken epoxy group and much more Nano-Ti is formed to promote the grafting reaction between Nano-Ti and epoxy resin. The results from TEM and XPS also prove that. And the grafting ration is maximum as the milling time is 240 min, the mass loss ratio is 17.53%.

Ball milling pretreatment of corn stover for enhancing the efficiency of enzymatic hydrolysis.

PubMed

Lin, Zengxiang; Huang, He; Zhang, Hongman; Zhang, Lin; Yan, Lishi; Chen, Jingwen

2010-11-01

Ethanol can be produced from lignocellulosic biomass with the usage of ball milling pretreatment followed by enzymatic hydrolysis and fermentation. The sugar yields from lignocellulosic feed stocks are critical parameters for ethanol production process. The research results from this paper indicated that the yields of glucose and xylose were improved by adding any of the following dilute chemical reagents: H(2)SO(4), HCl, HNO(3), CH(3)COOH, HCOOH, H(3)PO(4), and NaOH, KOH, Ca(OH)(2), NH(3)·H(2)O in the ball milling pretreatment of corn stover. The optimal enzymatic hydrolysis efficiencies were obtained under the conditions of ball milling in the alkali medium that was due to delignification. The data also demonstrated that ball milling pretreatment was a robust process. From the microscope image of ball milling-pretreated corn stover, it could be observed that the particle size of material was decreased and the fiber structure was more loosely organized. Meanwhile, the results indicate that the treatment effect of wet milling is better than that of dry milling. The optimum parameters for the milling process were ball speed of 350 r/min, solid/liquid ratio of 1:10, raw material particle size with 0.5 mm, and number of balls of 20 (steel ball, Φ = 10 mm), grinding for 30 min. In comparison with water milling process, alkaline milling treatment could increase the enzymatic hydrolysis efficiency of corn stover by 110%; and through the digestion process with the combination of xylanase and cellulase mixture, the hydrolysis efficiency could increase by 160%.

Mechanism of solid state amorphization of glucose upon milling.

PubMed

Dujardin, N; Willart, J F; Dudognon, E; Danède, F; Descamps, M

2013-02-07

Crystalline α-glucose is known to amorphize upon milling at -15 °C while it remains structurally invariant upon milling at room temperature. We have taken advantage of this behavior to compare the microstructural evolutions of the material in both conditions in order to identify the essential microstructural features which drive the amorphization process upon milling. The investigations have been performed by differential scanning calorimetry and by powder X-ray diffraction. The results indicate that two different amorphization mechanisms occur upon milling: an amorphization at the surface of crystallites due to the mechanical shocks and a spontaneous amorphization of the crystallites as they reach a critical size, which is close to 200 Å in the particular case of α-glucose.

Transformations in oxides induced by high-energy ball-milling.

PubMed

Šepelák, Vladimir; Bégin-Colin, Sylvie; Le Caër, Gérard

2012-10-21

This paper, by no means exhaustive, focuses on high-energy ball-milling of oxides, on their mechanically induced changes and on the consequences of such changes on their physical and chemical properties. High-energy ball-milling offers a fortunate combination of technical simplicity and of complexity both of physical mechanisms which act during milling and of mechanosynthesized materials. Its basic interest, which stems from the large diversity of routes it offers to prepare oxides either directly or indirectly, is illustrated with various families of oxides. The direct path is to be favoured when as-milled oxides are of interest per se because of their nanocrystalline characteristics, their defects or their modified structures which result from mechanically driven phase transformations. The indirect path consists of a sequence of steps starting with mechanically activated oxides which may be subsequently just annealed or submitted to a combination of thermal treatments, with the possible occurrence of various chemical reactions, to prepare the sought-after materials with potential gains in processing temperatures and times. High energy ball-milling of oxides is more and more currently used to activate powders and to prepare nano-oxides at moderate temperatures. The interest of an activation step is well illustrated by the broad development of doped titania powders, synthesized by heat treatment of pre-ground reactants, for photocatalytic applications or to develop antibacterial materials. Another important class of applications of high-energy ball-milling is the formation of composites. It is exemplified here with the case of oxide-dispersed strengthened alloys whose properties are considerably improved by a dispersion of ultra-stable nanosized oxides whose formation mechanisms were recently described. The basic understanding of the mechanisms by which oxides or oxide mixtures evolve by high-energy ball-milling appears to be less advanced than it is for metallic

Ball Milling Assisted Solvent and Catalyst Free Synthesis of Benzimidazoles and Their Derivatives.

PubMed

El-Sayed, Taghreed H; Aboelnaga, Asmaa; Hagar, Mohamed

2016-08-24

Benzoic acid and o-phenylenediamine efficiently reacted under the green solvent-free Ball Milling method. Several reaction parameters were investigated such as rotation frequency; milling balls weight and milling time. The optimum reaction condition was milling with 56.6 g weight of balls at 20 Hz frequency for one hour milling time. The study was extended for synthesis of a series of benzimidazol-2-one or benzimidazol-2-thione using different aldehydes; carboxylic acids; urea; thiourea or ammonium thiocyanate with o-phenylenediamine. Moreover; the alkylation of benzimidazolone or benzimidazolthione using ethyl chloroacetate was also studied.

Homogeneity of ball milled ceramic powders: Effect of jar shape and milling conditions.

PubMed

Broseghini, M; D'Incau, M; Gelisio, L; Pugno, N M; Scardi, P

2017-02-01

This paper contains data and supporting information of and complementary to the research article entitled " Effect of jar shape on high-energy planetary ball milling efficiency: simulations and experiments " (Broseghini et al.,) [1]. Calcium fluoride (CaF 2 ) was ground using two jars of different shape (cylindrical and half-moon) installed on a planetary ball-mill, exploring different operating conditions (jar-to-plate angular velocity ratio and milling time). Scanning Electron Microscopy (SEM) images and X-Ray Powder Diffraction data (XRPD) were collected to assess the effect of milling conditions on the end-product crystallite size. Due to the inhomogeneity of the end product, the Whole Powder Pattern Model (WPPM, (Scardi, 2008) [2]) analysis of XRPD data required the hypothesis of a bimodal distribution of sizes - respectively ground (fine fraction) and less-to-not ground (coarse fraction) - confirmed by SEM images and suggested by the previous literature (Abdellatief et al., 2013) [3,4]. Predominance of fine fraction clearly indicates optimal milling conditions.

Effects of ball-milling on lithium insertion into multi-walled carbon nanotubes synthesized by thermal chemical vapour deposition

NASA Astrophysics Data System (ADS)

Eom, JiYong; Kim, DongYung; Kwon, HyukSang

The effects of ball-milling on Li insertion into multi-walled carbon nanotubes (MWNTs) are presented. The MWNTs are synthesized on supported catalysts by thermal chemical vapour deposition, purified, and mechanically ball-milled by the high energy ball-milling. The purified MWNTs and the ball-milled MWNTs were electrochemically inserted with Li. Structural and chemical modifications in the ball-milled MWNTs change the insertion-extraction properties of Li ions into/from the ball-milled MWNTs. The reversible capacity (C rev) increases with increasing ball-milling time, namely, from 351 mAh g -1 (Li 0.9C 6) for the purified MWNTs to 641 mAh g -1 (Li 1.7C 6) for the ball-milled MWNTs. The undesirable irreversible capacity (C irr) decreases continuously with increase in the ball-milling time, namely, from 1012 mAh g -1 (Li 2.7C 6) for the purified MWNTs to 518 mAh g -1 (Li 1.4C 6) for the ball-milled MWNTs. The decrease in C irr of the ball-milled samples results in an increase in the coulombic efficiency from 25% for the purified samples to 50% for the ball-milled samples. In addition, the ball-milled samples maintain a more stable capacity than the purified samples during charge-discharge cycling.

Effect of milling conditions on solid-state amorphization of glipizide, and characterization and stability of solid forms.

PubMed

Xu, Kailin; Xiong, Xinnuo; Zhai, Yuanming; Wang, Lili; Li, Shanshan; Yan, Jin; Wu, Di; Ma, Xiaoli; Li, Hui

2016-09-10

In this study, the amorphization of glipizide was systematically investigated through high-energy ball milling at different temperatures. The results of solid-state amorphization through milling indicated that glipizide underwent direct crystal-to-glass transformation at 15 and 25°C and crystal-to-glass-to-crystal conversion at 35°C; hence, milling time and temperature had significant effects on the amorphization of glipizide, which should be effectively controlled to obtain totally amorphous glipizide. Solid forms of glipizide were detailedly characterized through analyses of X-ray powder diffraction, morphology, thermal curves, vibrational spectra, and solid-state nuclear magnetic resonance. The physical stability of solid forms was investigated under different levels of relative humidity (RH) at 25°C. Forms I and III are kinetically stable and do not form any new solid-state forms at various RH levels. By contrast, Form II is kinetically unstable, undergoing direct glass-to-crystal transformation when RH levels higher than 32.8%. Therefore, stability investigation indicated that Form II should be stored under relatively dry conditions to prevent rapid crystallization. High temperatures can also induce the solid-state transformation of Form II; the conversion rate increased with increasing temperature. Copyright © 2016 Elsevier B.V. All rights reserved.

Structure and electrochemical behaviour of metastable Mg 50Ti 50 alloy prepared by ball milling

NASA Astrophysics Data System (ADS)

Rousselot, S.; Bichat, M.-P.; Guay, D.; Roué, L.

A 50-50 mixture of Mg and Ti was milled for different times, and the cycling discharge capacities of the resulting compounds were evaluated in KOH media. From Rietveld refinement analysis of the X-ray diffraction patterns, it is shown that a metastable hcp Mg 50Ti 50 compound is formed after 20 h of milling. This material has a very low-electrochemical hydriding activity. However, in the presence of 10 wt.% Pd (added before milling), it displays a maximum discharge capacity of ca. 400 mAh g -1 after three charge/discharge cycles. The irreversible structural evolution of the Mg 50Ti 50 alloy from a hcp phase to a fcc phase upon cycling is demonstrated.

Ball milling pretreatment of oil palm biomass for enhancing enzymatic hydrolysis.

PubMed

Zakaria, Mohd Rafein; Fujimoto, Shinji; Hirata, Satoshi; Hassan, Mohd Ali

2014-08-01

Oil palm biomass, namely empty fruit bunch and frond fiber, were pretreated using a planetary ball mill. Particle sizes and crystallinity index values of the oil palm biomass were significantly reduced with extended ball mill processing time. The treatment efficiency was evaluated by the generation of glucose, xylose, and total sugar conversion yields from the pretreatment process compared to the amount of sugars from raw materials. Glucose and xylose contents were determined using high-performance liquid chromatography. An increasing trend in glucose and xylose yield as well as total sugar conversion yield was observed with decreasing particle size and crystallinity index. Oil palm frond fiber exhibited the best material yields using ball milling pretreatment with generated glucose, xylose, and total sugar conversion yields of 87.0, 81.6, and 85.4%, respectively. In contrast, oil palm empty fruit bunch afforded glucose and xylose of 70.0 and 82.3%, respectively. The results obtained in this study showed that ball mill-treated oil palm biomass is a suitable pretreatment method for high conversion of glucose and xylose.

Preparation of ultrafine magnetic biochar and activated carbon for pharmaceutical adsorption and subsequent degradation by ball milling.

PubMed

Shan, Danna; Deng, Shubo; Zhao, Tianning; Wang, Bin; Wang, Yujue; Huang, Jun; Yu, Gang; Winglee, Judy; Wiesner, Mark R

2016-03-15

Ball milling was used to prepare two ultrafine magnetic biochar/Fe3O4 and activated carbon (AC)/Fe3O4 hybrid materials targeted for use in pharmaceutical removal by adsorption and mechanochemical degradation of pharmaceutical compounds. Both hybrid adsorbents prepared after 2h milling exhibited high removal of carbamazepine (CBZ), and were easily separated magnetically. These adsorbents exhibited fast adsorption of CBZ and tetracycline (TC) in the initial 1h. The biochar/Fe3O4 had a maximum adsorption capacity of 62.7mg/g for CBZ and 94.2mg/g for TC, while values obtained for AC/Fe3O4 were 135.1mg/g for CBZ and 45.3mg/g for TC respectively when data were fitted using the Langmuir expression. Solution pH values slightly affected the sorption of TC on the adsorbents, while CBZ sorption was almost pH-independent. The spent adsorbents with adsorbed CBZ and TC were milled to degrade the adsorbed pollutants. The adsorbed TC itself was over 97% degraded after 3h of milling, while about half of adsorbed CBZ were remained. The addition of quartz sand was found to improve the mechanochemical degradation of CBZ on biochar/Fe3O4, and its degradation percent was up to 98.4% at the dose of 0.3g quarts sand/g adsorbent. This research provided an easy method to prepare ultrafine magnetic adsorbents for the effective removal of typical pharmaceuticals from water or wastewater and degrade them using ball milling. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of ultrafine magnetic biochar and activated carbon for pharmaceutical adsorption and subsequent degradation by ball milling

PubMed Central

Shan, Danna; Deng, Shubo; Zhao, Tianning; Wang, Bin; Wang, Yujue; Huang, Jun; Yu, Gang; Winglee, Judy; Wiesner, Mark R.

2017-01-01

Ball milling was used to prepare two ultrafine magnetic biochar/Fe3O4 and activated carbon (AC)/Fe3O4 hybrid materials targeted for use in pharmaceutical removal by adsorption and mechanochemical degradation of pharmaceutical compounds. Both hybrid adsorbents prepared after 2 hours milling exhibited high removal of carbamazepine (CBZ), and were easily separated magnetically. These adsorbents exhibited fast adsorption of CBZ and tetracycline (TC) in the initial 1 hour. The biochar/Fe3O4 had a maximum adsorption capacity of 62.7 mg/g for CBZ and 94.2 mg/g for TC, while values obtained for AC/Fe3O4 were 135.1 mg/g for CBZ and 45.3 mg/g for TC respectively when data were fitted using the Langmuir expression. Solution pH values slightly affected the sorption of TC on the adsorbents, while CBZ sorption was almost pH-independent. The spent adsorbents with adsorbed CBZ and TC were milled to degrade the adsorbed pollutants. The adsorbed TC itself was over 97% degraded after 3 hours of milling, while about half of adsorbed CBZ were remained. The addition of quartz sand was found to improve the mechanochemical degradation of CBZ on biochar/Fe3O4, and its degradation percent was up to 98.4% at the dose of 0.3 g quarts sand/g adsorbent. This research provided an easy method to prepare ultrafine magnetic adsorbents for the effective removal of typical pharmaceuticals from water or wastewater and degrade them using ball milling. PMID:26685062

Raman spectroscopy fingerprint of stainless steel-MWCNTs nanocomposite processed by ball-milling

NASA Astrophysics Data System (ADS)

dos Reis, Marcos Allan Leite; Barbosa Neto, Newton Martins; de Sousa, Mário Edson Santos; Araujo, Paulo T.; Simões, Sónia; Vieira, Manuel F.; Viana, Filomena; Loayza, Cristhian R. L.; Borges, Diego J. A.; Cardoso, Danyella C. S.; Assunção, Paulo D. C.; Braga, Eduardo M.

2018-01-01

Stainless steel 304L alloy powder and multiwalled carbon nanotubes were mixed by ball-milling under ambient atmosphere and in a broad range of milling times, which spans from 0 to 120 min. Here, we provided spectroscopic signatures for several distinct composites produced, to show that the Raman spectra present interesting splittings of the D-band feature into two main sub-bands, D-left and D-right, together with several other secondary features. The G-band feature also presents multiple splittings that are related to the outer and inner diameter distributions intrinsic to the multiwalled carbon nanotube samples. A discussion about the second order 2D-band (also known as G'-band) is also provided. The results reveal that the multiple spectral features observed in the D-band are related to an increased chemical functionalization. A lower content of amorphous carbon at 60 and 90 min of milling time is verified and the G-band frequencies associated to the tubes in the outer diameters distribution is upshifted, which suggests that doping induced by strain is taking place in the milled samples. The results indicate that Raman spectroscopy can be a powerful tool for a fast and non-destructive characterization of carbon nanocomposites used in powder metallurgy manufacturing processes.

Mechanochemical destruction of mirex co-ground with iron and quartz in a planetary ball mill.

PubMed

Yu, Yunfei; Huang, Jun; Zhang, Wang; Zhang, Kunlun; Deng, Shubo; Yu, Gang

2013-02-01

Mechanochemical destruction (MCD) has been recognized as a promising non-combustion technology for the disposal of obsolete pesticides belonging to the persistent organic pollutants (POPs). Mirex, a termiticide ever used for many years in China, was ball milled in the presence of various reagent(s) in a planetary ball mill at room temperature to investigate the destruction efficiency. The ground samples were characterized and analyzed by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, gas chromatography (GC), and ion chromatography (Martins, Bicego et al.). Under the same conditions of mill rotary rate and charge ratio, the mixture of iron powder and quartz sand (Fe/SiO(2)) was found best in promoting the mirex destruction. Mirex was completed destroyed after 2 h grinding at a charge ratio of 36:1 (reagent/mirex, m/m) and a mill rotation speed of 550 rpm. No organic compound was detected by GC/μECD screening. The yield of water-soluble chlorine determined by ion chromatography (Martins, Bicego et al.) in the final residue accounted for 90.7% of chlorine in the original mirex, which indicated a nearly complete dechlorination. Signals of both graphite and amorphous carbon were found in the Raman spectra of the co-ground powder samples. With the main final degradation products of water soluble Cl and carbon, the mechanism of the mechanochemical destruction approach should be dechlorination followed by the carbonization. Copyright © 2012 Elsevier Ltd. All rights reserved.

MgO-based adsorbents for CO2 adsorption: Influence of structural and textural properties on the CO2 adsorption performance.

PubMed

Elvira, Gutiérrez-Bonilla; Francisco, Granados-Correa; Víctor, Sánchez-Mendieta; Alberto, Morales-Luckie Raúl

2017-07-01

A series of MgO-based adsorbents were prepared through solution-combustion synthesis and ball-milling process. The prepared MgO-based powders were characterized using X-ray diffraction, scanning electron microscopy, N 2 physisorption measurements, and employed as potential adsorbents for CO 2 adsorption. The influence of structural and textural properties of these adsorbents over the CO 2 adsorption behaviour was also investigated. The results showed that MgO-based products prepared by solution-combustion and ball-milling processes, were highly porous, fluffy, nanocrystalline structures in nature, which are unique physico-chemical properties that significantly contribute to enhance their CO 2 adsorption. It was found that the MgO synthesized by solution combustion process, using a molar ratio of urea to magnesium nitrate (2:1), and treated by ball-milling during 2.5hr (MgO-BM2.5h), exhibited the maximum CO 2 adsorption capacity of 1.611mmol/g at 25°C and 1atm, mainly via chemisorption. The CO 2 adsorption behaviour on the MgO-based adsorbents was correlated to their improved specific surface area, total pore volume, pore size distribution and crystallinity. The reusability of synthesized MgO-BM2.5h was confirmed by five consecutive CO 2 adsorption-desorption times, without any significant loss of performance, that supports the potential of MgO-based adsorbent. The results confirmed that the special features of MgO prepared by solution-combustion and treated by ball-milling during 2.5hr are favorable to be used as effective MgO-based adsorbent in post-combustion CO 2 capture technologies. Copyright © 2016. Published by Elsevier B.V.

The Tool Life of Ball Nose end Mill Depending on the Different Types of Ramping

NASA Astrophysics Data System (ADS)

Vopát, Tomáš; Peterka, Jozef; Kováč, Martin

2014-12-01

The article deals with the cutting tool wear measurement process and tool life of ball nose end mill depending on upward ramping and downward ramping. The aim was to determine and compare the wear (tool life) of ball nose end mill for different types of copy milling operations, as well as to specify particular steps of the measurement process. In addition, we examined and observed cutter contact areas of ball nose end mill with machined material. For tool life test, DMG DMU 85 monoBLOCK 5-axis CNC milling machine was used. In the experiment, cutting speed, feed rate, axial depth of cut and radial depth of cut were not changed. The cutting tool wear was measured on Zoller Genius 3s universal measuring machine. The results show different tool life of ball nose end mills depending on the copy milling strategy.

High energy ball milling and supercritical carbon dioxide impregnation as co-processing methods to improve dissolution of tadalafil.

PubMed

Krupa, Anna; Descamps, Marc; Willart, Jean-François; Jachowicz, Renata; Danède, Florence

2016-12-01

Tadalafil (TD) is a crystalline drug of a high melting point (T m =299°C) and limited solubility in water (<5μg/mL). These properties may result in reduced and variable bioavailability after oral administration. Since the melting of TD is followed by its decomposition, the drug processing at high temperatures is limited. The aim of the research is, therefore, to improve the dissolution of TD by its co-processing with the hydrophilic polymer Soluplus® (SL) at temperatures below 40°C. In this study, two methods, i.e. high energy ball-milling and supercritical carbon dioxide impregnation (scCO 2 ) are compared, with the aim to predict their suitability for the vitrification of TD. The influence of the amount of SL and the kind of co-processing method on TD thermal properties is analyzed. The results show that only the high energy ball milling process makes it possible to obtain a completely amorphous form of TD, with the characteristic X-ray 'halo' pattern. The intensity of the Bragg peaks diminishes for all the formulations treated with scCO 2 , but these samples remain crystalline. The MDSC results show that high energy ball milling is capable of forcing the mixing of TD and SL at a molecular level, providing a homogeneous amorphous solid solution. The glass transition temperatures (T g ), determined for the co-milled formulations, range from 79°C to 139°C and they are higher than T g of pure SL (ca. 70°C) and lower than T g of pure TD (ca. 149°C). In contrast to the co-milled formulations which are in the form of powder, all the formulations after scCO 2 impregnation form a hard residue, sticking to the reaction vessel, which needs to be ground before analysis or further processing. Finally, the dissolution studies show that not only has SL a beneficial effect on the amount of TD dissolved, but also both co-processing methods make the dissolution enhancement of TD possible. After co-processing by scCO 2 , the amount of TD dissolved increases with the

Microstructure-Property Correlation in Magnesium-based Hydrogen Storage Systems: The Case for Ball-milled Magnesium Hydride Powder and Magnesium-based Multilayered Composites

NASA Astrophysics Data System (ADS)

Danaie, Mohsen

The main focus of this thesis is the characterization of defects and microstructure in high-energy ball milled magnesium hydride powder and magnesium-based multilayered composites. Enhancement in kinetics of hydrogen cycling in magnesium can be achieved by applying severe plastic deformation. A literature survey reveals that, due to extreme instability of alpha-MgH 2 in transmission electron microscope (TEM), the physical parameters that researchers have studied are limited to particle size and grain size. By utilizing a cryogenic TEM sample holder, we extended the stability time of the hydride phase during TEM characterization. Milling for only 30 minutes resulted in a significant enhancement in desorption kinetics. A subsequent annealing cycle under pressurized hydrogen reverted the kinetics to its initial sluggish state. Cryo-TEM analysis of the milled hydride revealed that mechanical milling induces deformation twinning in the hydride microstructure. Milling did not alter the thermodynamics of desorption. Twins can enhance the kinetics by acting as preferential locations for the heterogeneous nucleation of metallic magnesium. We also looked at the phase transformation characteristics of desorption in MgH2. By using energy-filtered TEM, we investigated the morphology of the phases in a partially desorbed state. Our observations prove that desorption phase transformation in MgH2 is of "nucleation and growth" type, with a substantial energy barrier for nucleation. This is contrary to the generally assumed "core-shell" structure in most of the simulation models for this system. We also tested the hydrogen storage cycling behavior of bulk centimeter-scale Mg-Ti and Mg-SS multilayer composites synthesized by accumulative roll-bonding. Addition of either phase (Ti or SS) allows the reversible hydrogen sorption at 350°C, whereas identically roll-bonded pure magnesium cannot be absorbed. In the composites the first cycle of absorption (also called "activation

Contamination Effects on Improving the Hydrogenation/Dehydrogenation Kinetics of Binary Magnesium Hydride/Titanium Carbide Systems Prepared by Reactive Ball Milling

PubMed Central

El-Eskandarany, M. Sherif; Shaban, Ehab

2015-01-01

Ultrafine MgH2 nanocrystalline powders were prepared by reactive ball milling of elemental Mg powders after 200 h of high-energy ball milling under a hydrogen gas pressure of 50 bar. The as-prepared metal hydride powders were contaminated with 2.2 wt. % of FeCr-stainless steel that was introduced to the powders upon using stainless steel milling tools made of the same alloy. The as-synthesized MgH2 was doped with previously prepared TiC nanopowders, which were contaminated with 2.4 wt. % FeCr (materials of the milling media), and then ball milled under hydrogen gas atmosphere for 50 h. The results related to the morphological examinations of the fabricated nanocomposite powders beyond the micro-and nano-levels showed excellent distributions of 5.2 wt. % TiC/4.6 wt. % FeCr dispersoids embedded into the fine host matrix of MgH2 powders. The as-fabricated nanocomposite MgH2/5.2 wt. % TiC/4.6 wt. % FeCr powders possessed superior hydrogenation/dehydrogenation characteristics, suggested by the low value of the activation energy (97.74 kJ/mol), and the short time required for achieving a complete absorption (6.6 min) and desorption (8.4 min) of 5.51 wt. % H2 at a moderate temperature of 275 °C under a hydrogen gas pressure ranging from 100 mbar to 8 bar. van’t Hoff approach was used to calculate the enthalpy (∆H) and entropy (∆S) of hydrogenation for MgH2, which was found to be −72.74 kJ/mol and 112.79 J/mol H2/K, respectively. Moreover, van’t Hoff method was employed to calculate the ΔH and ΔS of dehydrogenation, which was found to be 76.76 kJ/mol and 119.15 J/mol H2/K, respectively. This new nanocomposite system possessed excellent absorption/desorption cyclability of 696 complete cycles, achieved in a cyclic-life-time of 682 h. PMID:28793606

The Effect of High Energy Ball Milling on the Dynamic Response of Aluminum Powders

NASA Astrophysics Data System (ADS)

Beason, Matthew T.; Justice, Andrew W.; Gunduz, Ibrahim E.; Son, Steven F.

2017-06-01

Ball milling is an effective method to enhance the reactivity of intermetallic reactives by reducing characteristic diffusions distances. During this process, ductile reactants are mixed into a lamellar material with nanoscale features, resulting in significant strain hardening. Plate impact experiments using a single stage light gas gun have been performed to evaluate the effect of high energy ball milling (HEBM) on the mechanical properties and dynamic response of cold pressed aluminum compacts. The average grain size of the milled material is evaluate and suggested as a method of correlating the measured response to the properties of milled composites. This material is based upon work supported by the Department of Energy, National Nuclear Security Administration, under Award Number(s) DE-NA0002377, as well as individual funding (Beason) by the Department of Defense through the NDSEG.

Discrete element method based scale-up model for material synthesis using ball milling

NASA Astrophysics Data System (ADS)

Santhanam, Priya Radhi

depending on hardness of brittle component relative to milling media. To improve the DEM model of the attritor mill, it is desired to avoid the removal of unrealistic, high-force events using an approach that would not predict such events in the first place. It is observed that during experiments in attritor, balls may jam causing an increased resistance to the impeller's rotation. The impeller may instantaneously slow down, quickly returning to its pre-set rotation rate. Previous DEM models did not account for such rapid changes in the impeller's rotation. In this work, this relationship between impeller's torque and rotation rate is obtained experimentally and introduced in DEM. As a result, predicted Ed, are shown to correlate well with the experimental data. Finally, a methodology is proposed combining an experiment and its DEM description enabling one to identify the appropriate interaction parameters for powder systems. The experiment uses a miniature vibrating hopper and can be applied to characterize the powder flow for variety of materials. The hopper is designed to hold up to 20,000 particles of 50-mum diameter, which can be directly described in DEM. Based on comparison of discharge rate from experiments and model, all 6 interaction parameters were analyzed and the ideal conditions identified for Zirconia beads. The values of these parameters for powders are generally not the same as those established for macroscopic bodies. In addition, effects of some other experimental parameters such as particle size distribution and amplitude of vibration are also investigated.

Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.

The study on dynamic properties of monolithic ball end mills with various slenderness

NASA Astrophysics Data System (ADS)

Wojciechowski, Szymon; Tabaszewski, Maciej; Krolczyk, Grzegorz M.; Maruda, Radosław W.

2017-10-01

The reliable determination of modal mass, damping and stiffness coefficient (modal parameters) for the particular machine-toolholder-tool system is essential for the accurate estimation of vibrations, stability and thus the machined surface finish formed during the milling process. Therefore, this paper focuses on the analysis of ball end mill's dynamical properties. The tools investigated during this study are monolithic ball end mills with different slenderness values, made of coated cemented carbide. These kinds of tools are very often applied during the precise milling of curvilinear surfaces. The research program included the impulse test carried out for the investigated tools clamped in the hydraulic toolholder. The obtained modal parameters were further applied in the developed tool's instantaneous deflection model, in order to estimate the tool's working part vibrations during precise milling. The application of the proposed dynamics model involved also the determination of instantaneous cutting forces on the basis of the mechanistic approach. The research revealed that ball end mill's slenderness can be considered as an important milling dynamics and machined surface quality indicator.

Ball mill tool for crushing coffee and cocoa beans base on fraction size sieving results

NASA Astrophysics Data System (ADS)

Haryanto, B.; Sirait, M.; Azalea, M.; Alvin; Cahyani, S. E.

2018-02-01

Crushing is one of the operation units that aimed to convert the size of solid material to be smoother particle’s size. The operation unit that can be used in this crushing is ball mill. The purpose of this study is to foresee the effect of raw material mass, grinding time, and the number of balls that are used in the ball mill tool related to the amount of raw material of coffee and cocoa beans. Solid material that has become smooth is then sieved with sieve mesh with size number: 50, 70, 100, and 140. It is in order to obtain the mass fraction that escaped from each sieve mesh. From the experiment, it can be concluded that mass percentage fraction of coffee powder is bigger than cocoa powder that escaped from the mesh. Hardness and humidity of coffee beans and cocoa beans have been the important factors that made coffee beans is easier to be crushed than cocoa beans.

Matrix model of the grinding process of cement clinker in the ball mill

NASA Astrophysics Data System (ADS)

Sharapov, Rashid R.

2018-02-01

In the article attention is paid to improving the efficiency of production of fine powders, in particular Portland cement clinker. The questions of Portland cement clinker grinding in closed circuit ball mills. Noted that the main task of modeling the grinding process is predicting the granulometric composition of the finished product taking into account constructive and technological parameters used ball mill and separator. It is shown that the most complete and informative characterization of the grinding process in a ball mill is a grinding matrix taking into account the transformation of grain composition inside the mill drum. Shows how the relative mass fraction of the particles of crushed material, get to corresponding fraction. Noted, that the actual task of reconstruction of the matrix of grinding on the experimental data obtained in the real operating installations. On the basis of experimental data obtained on industrial installations, using matrix method to determine the kinetics of the grinding process in closed circuit ball mills. The calculation method of the conversion of the grain composition of the crushed material along the mill drum developed. Taking into account the proposed approach can be optimized processing methods to improve the manufacturing process of Portland cement clinker.

Study of Initial Stages of Ball-Milling of Cu Powder Using X-ray Diffraction

NASA Astrophysics Data System (ADS)

Gayathri, N.; Mukherjee, Paramita

2018-04-01

The initial stage of size refinement of Cu powder is studied using detailed X-ray diffraction (XRD) analysis to understand the mechanism of formation of nanomaterials during the ball-milling process. The study was restricted to samples obtained for milling time up to 240 min to understand the deformation mechanism at the early stages of ball milling. Various model based approaches for the analysis of the XRD were used to study the evolution of the microstructural parameters such as domain size and microstrain along the different crystallographic planes. It was seen that the domain size saturates at a low value along the (311) plane whereas the size along the (220) and (200) plane is still higher. The r.m.s microstrain showed a non-monotonic change along the different crystallographic directions up to the milling time of 240 min.

The effect of milling time on the synthesis of Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kursun, C., E-mail: celalkursun@ksu.edu.tr; Gogebakan, M., E-mail: gogebakan@ksu.edu.tr

In the present work, nanocrystalline Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy was produced by mechanical alloying from mixtures of pure crystalline Cu, Mg, Ti and Ni powders using a Fritsch planetary ball mill with a ball to powder ratio of 10:1. Morphological changes, microstructural evolution and thermal behaviour of the Cu-Mg-Ti-Ni powders at different stages of milling were characterised by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) and differential thermal analysis (DTA). This alloy resulted in formation of single phase solid solution with FCC structure α-Cu (Mg, Ti, Ni) after 80 h of milling. In the initialmore » stage of milling different sized and shaped elemental powders became uniform during mechanical alloying. The homogeneity of the Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy increased with increasing milling time. The EDX result also confirmed the compositional homogeneity of the powder alloy. The crystallite size of alloy was calculated below 10 nm from XRD data.« less

Effect of ball milling and heat treatment process on MnBi powders magnetic properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xie, Wei; Polikarpov, Evgueni; Choi, Jung-Pyung

The metallic compound MnBi has high intrinsic coercivity with large positive temperature coefficient. The coercivity of MnBi exceeds 12 kOe and 26 kOe at 300 K and 523 K, respectively. Hence MnBi is a good candidate for the hard phase in exchange coupled nanocomposite magnets. In order to maximize the loading of the soft phase, the size of the MnBi particle has to be close to 500 nm, the size of single magnetic domain. Low energy milling is the common method to reduce MnBi particle size. However, only 3-7 mu m size particle can be achieved without significant decomposition. Here,more » we report our effort on preparing submicron MnBi powders using traditional powder metallurgy methods. Mn55Bi45 magnetic powders were prepared using arc melting method, followed by a series of thermal-mechanical treatment to improve purity, and finished with low energy ball milling at cryogenic temperature to achieve submicron particle size. The Mn55Bi45 powders were decomposed during ball milling process and recovered during 24 h 290 degrees C annealing process. With increasing ball-milling time, the saturation magnetization of MnBi decreases, while the coercivity increases. Annealing after ball milling recovers some of the magnetization, indicating the decomposition occurred during the ball-milling process can be reversed. The coercivity of Mn55Bi45 powders are also improved as a result of the heat treatment at 290 degrees C for 24 h. The world record magnetization 71.2 emu/g measured applying a field of 23 kOe has been achieved via low energy ball mill at room temperature« less

Amorphization of Indomethacin by Co-Grinding with Neusilin US2: amorphization kinetics, physical stability and mechanism.

PubMed

Bahl, Deepak; Bogner, Robin H

2006-10-01

To quantify the effects of the ratio of indomethacin to Neusilin US2 and the processing humidity on the amorphization kinetics, stability and nature of the interaction. A porcelain jar mill with zirconia balls was used to affect conversion of the physical mixtures (48 g) of indomethacin and Neusilin US2 (in the ratios 1:1 to 1:5) to amorphous states at room temperature (25 degrees C) employing either 0% RH or 75% RH. The percent crystallinity in the samples was determined from ATR-FTIR scans chemometrically. The physical stability of these co-ground amorphous powders was evaluated at 40 degrees C/75% RH and 40 degrees C/0% RH. The lower the ratio of indomethacin to Neusilin US2, the faster is the amorphization during co-grinding. Higher humidity facilitates amorphization with a more pronounced effect at the lower ratio of indomethacin to Neusilin US2. There is further amorphization of some of the partially amorphized samples on storage at 40 degrees C/75% RH for 3 months. Hydrogen bonding and surface interaction between metal ions of Neusilin US2 and indomethacin can explain changes in the FTIR spectra. The processing humidity and the ratio of indomethacin to Neusilin US2 are important factors to be considered to affect amorphization during ball milling. Amorphous indomethacin can be stabilized by co-grinding with Neusilin US2.

Preparation of Si nano-crystals with controlled oxidation state from SiO disproportionated by ZrO2 ball-milling

NASA Astrophysics Data System (ADS)

Okamoto, Yuji; Harada, Yoshitomo; Ohta, Narumi; Takada, Kazunori; Sumiya, Masatomo

2016-09-01

We demonstrate that a SiO disproportionation reaction can be achieved simply by high energy mechanochemical milling. The planetary ball-milling of ZrO2 for a few minutes generated Si nano-crystals. Milling conditions including rotation speed, ball number, milling time, and type of ball material were able to control the oxidation states of Si. The ball-milled SiO powder was tested as an anode of a lithium battery. ZrO2 contamination from the vial and balls was eliminated by dipping the ball-milled SiO powder in (NH4)HSO4 molten salt and heating for 5 min. The disproportionated SiO powder showed characteristics comparable to those of a powder prepared by a conventional heating process taking several hours.

Ball milling: An experimental support to the energy transfer evaluated by the collision model

DOE Office of Scientific and Technical Information (OSTI.GOV)

Magini, M.; Iasonna, A.; Padella, F.

1996-01-01

In recent years several attempts have been made in order to understand the fundamentals of the ball milling process. The aim of these approaches is to establish predictive capabilities for this process, i.e. the possibility of obtaining a given product by suitable choosing the proper milling conditions. Maurice and Courtney have modeled ball milling in a planetary and in a vibratory mill including parameters like impact times, areas of the colliding surfaces (derived from hertzian collision theory), powder strain rates and pressure peak during collision. Burgio et al derived the kinematic equations of a ball moving on a planetary millmore » and the consequent ball-to-powder energy transfer occurring in a single collision event. The fraction of input energy transferred to the powder was subsequently estimated by an analysis of the collision event. Finally an energy map was constructed which was the basis for a model with predictive capabilities. The aim of the present article is to show that the arguments used to construct the model of the milling process has substantial experimental support.« less

Defect induced electronic states and magnetism in ball-milled graphite.

PubMed

Milev, Adriyan; Dissanayake, D M A S; Kannangara, G S K; Kumarasinghe, A R

2013-10-14

The electronic structure and magnetism of nanocrystalline graphite prepared by ball milling of graphite in an inert atmosphere have been investigated using valence band spectroscopy (VB), core level near-edge X-ray absorption fine structure (NEXAFS) spectroscopy and magnetic measurements as a function of the milling time. The NEXAFS spectroscopy of graphite milled for 30 hours shows simultaneous evolution of new states at ~284.0 eV and at ~290.5 eV superimposed upon the characteristic transitions at 285.4 eV and 291.6 eV, respectively. The modulation of the density of states is explained by evolution of discontinuities within the sheets and along the fracture lines in the milled graphite. The magnetic measurements in the temperature interval 2-300-2 K at constant magnetic field strength show a correlation between magnetic properties and evolution of the new electronic states. With the reduction of the crystallite sizes of the graphite fragments, the milled material progressively changes its magnetic properties from diamagnetic to paramagnetic with contributions from both Pauli and Curie paramagnetism due to the evolution of new states at ~284 and ~290.5 eV, respectively. These results indicate that the magnetic behaviour of ball-milled graphite can be manipulated by changing the milling conditions.

Effect of ball-milling to the surface morphology of CaCO3

NASA Astrophysics Data System (ADS)

Sulimai, N. H.; Rani, Rozina Abdul; Khusaimi, Z.; Abdullah, S.; Salifairus, M. J.; Alrokayan, Salman; Khan, Haseeb; Rusop, M.

2018-05-01

Calcium Carbonate can be synthesized in many approaches. This work studied on the physical changes to Calcium Carbonate (CaCO3) by ball-milling activity in different parameters; number of ball; collision duration; revolution per minute (RPM). Zirconia balls were used in the work because it has the best durability to withstand ball-milling conditions set. Industrial grade CaCO3 particles that were run in aforementioned parameters were characterized by Field Emission Scanning Electron Microscope (FE-SEM) to study the physical changes on the size and surface of the CaCO3. They were also characterized with Fourier Transform Infra-red Spectroscopy (FTIR) were fingerprint of CaCO3 regions were identified and any changes in the band position and intensity were discussed. Number of Zirconia balls and collision duration is directly proportional to the absorbance intensity whereas it is inversely proportional for the rpm. The best number of parameters producing the highest Absorbance is 100 Zirconia balls in duration of 1 hour and 100rpm.

Effects of milling media on the fabrication of melt-derived bioactive glass powder for biomaterial application

NASA Astrophysics Data System (ADS)

Ibrahim, Nurul Farhana; Mohamad, Hasmaliza; Noor, Siti Noor Fazliah Mohd

2016-12-01

The present work aims to study the effects of using different milling media on bioactive glass produced through melt-derived method for biomaterial application. The bioactive glass powder based on SiO2-CaO-Na2O-P2O5 system was fabricated using two different types of milling media which are tungsten carbide (WC) and zirconia (ZrO2) balls. However, in this work, no P2O5 was added in the new composition. XRF analysis indicated that tungsten trioxide (WO3) was observed in glass powder milled using WC balls whereas ZrO2 was observed in glass powder milled using ZrO2 balls. Amorphous structure was detected with no crystalline peak observed through XRD analysis for both glass powders. FTIR analysis confirmed the formation of silica network with the existence of functional groups Si-O-Si (bend), Si-O-Si (tetrahedral) and Si-O-Si (stretch) for both glass powders. The results revealed that there was no significant effect of milling media on amorphous silica network glass structure which shows that WC and zirconia can be used as milling media for bioactive glass fabrication without any contamination. Therefore, the fabricated BG can be tested safely for bioactivity assessment in biological fluids environment.

Ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling

NASA Astrophysics Data System (ADS)

Bangi, Uzma K. H.; Park, Hyung-Ho; Han, Wooje; Prakshale, Vipul M.; Deshmukh, Lalasaheb P.

2017-05-01

The experimental results on the ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling have been reported in the present work. Lead oxide nanoflowers were prepared employing mixed ligands by subjecting the formed precipitate to ultrasonication and grinding/ball milling. The effect of ball milling as well as fine grinding in agate mortar on the microstructure and surface morphology of the lead oxide was studied. The characteristics of synthesized PbO were studied using X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and field emission scanning electron microscopy techniques. XRD results demonstrated the tetragonal phase of PbO with crystallite size of around 25 nm and strain of 3.6 × 10-3 calculated from Williamson-Hall plot. FESEM images manifested the formation of nanodiscs and nanoflowers with a diameter of around 300 nm and thickness of 50 nm. XPS spectra revealed the formation of PbO with photoelectron peak of Pb 4f and O 1 s lied at 137.68 and 529.96 eV. Moreover, FTIR spectrum exhibited Pb-O bond peak in the range of 400-530 cm-1.

Effect of ball milling time on thermoelectric properties of bismuth telluride nanomaterials

NASA Astrophysics Data System (ADS)

Khade, Poonam; Bagwaiya, Toshi; Bhattacharaya, Shovit; Singh, Ajay; Jha, Purushottam; Shelke, Vilas

2018-04-01

The effect of different milling time on thermoelectric properties of bismuth telluride (Bi2Te3) was investigated. The nanomaterial was prepared by varying the ball milling time and followed by hot press sintering. The crystal structure and phase formation were verified by X-ray diffraction and Raman Spectroscopy. The experimental results show that electrical conductivity increases whereas thermal conductivity decreases with increasing milling time. The negative sign of seebeck coefficient indicate the n-type nature with majority charge carriers of electrons. A maximum figure of merit about 0.55 is achieved for l5hr ball milled Bi2Te3 sample. The present study demonstrates the simple and cost-effective method for synthesis of Bi2Te3 thermoelectric material at large scale thermoelectric applications.

A co-production of sugars, lignosulfonates, cellulose, and cellulose nanocrystals from ball-milled woods

Treesearch

Lanxing Du; Jinwu Wang; Yang Zhang; Chusheng Qi; Michael P. Wolcott; Zhiming Yu

2017-01-01

This study demonstrated the technical potential for the large-scale co-production of sugars, lignosulfonates, cellulose, and cellulose nanocrystals. Ball-milled woods with two particle sizes were prepared by ball milling for 80 min or 120 min (BMW80, BMW120) and then enzymatically hydrolyzed. 78.3% cellulose conversion of...

Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling

PubMed Central

Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

2016-01-01

Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans (“dioxins”). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg−1) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg−1) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated. PMID:26975802

Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling

NASA Astrophysics Data System (ADS)

Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

2016-03-01

Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans (“dioxins”). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg-1) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg-1) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated.

Solid-state amorphization of rebamipide and investigation on solubility and stability of the amorphous form.

PubMed

Xiong, Xinnuo; Xu, Kailin; Li, Shanshan; Tang, Peixiao; Xiao, Ying; Li, Hui

2017-02-01

Solid-state amorphization of crystalline rebamipide (RBM) was realized by ball milling and spray drying. The amorphous content of samples milled for various time was quantified using X-ray powder diffraction. Crystalline RBM and three amorphous RBM obtained by milling and spray drying were characterized by morphological analysis, X-ray diffraction, thermal analysis and vibrational spectroscopy. The crystal structure of RBM was first determined by single-crystal X-ray diffraction. In addition, the solubility and dissolution rate of the RBM samples were investigated in different media. Results indicated that the solubility and the dissolution rates of spray-dried RBM-PVP in different media were highly improved compared with crystalline RBM. The physical stabilities of the three amorphous RBM were systematically investigated, and the stability orders under different storage temperatures and levels of relative humidity (RH) were both as follows: spray dried RBM < milled RBM < spray dried RBM-PVP. A direct glass-to-crystal transformation was induced under high RH, and the transformation rate rose with increasing RH. However, amorphous RBM could stay stable at RH levels lower than 57.6% (25 °C).

Comparison of characteristics of hydroxyapatite powders synthesized from cuttlefish bone via precipitation and ball milling techniques

NASA Astrophysics Data System (ADS)

Faksawat, K.; Kaewwiset, W.; Limsuwan, P.; Naemchanthara, K.

2017-09-01

The aim of this work was to compare characteristics of hydroxyapatite synthesized by precipitation and ball milling techniques. The cuttlefish bone powder was a precursor in calcium source and the di ammonium hydrogen orthophosphate powders was a precursor in phosphate source. The hydroxyapatite was synthesized by the both techniques such as precipitation and ball milling techniques. The phase formation, chemical structure and morphology of the both hydroxyapatite powders have been examined by X-ray diffractometer (XRD), Fourier transform infrared spectroscope (FTIR) and field emission scanning electron microscope (FESEM), respectively. The results show that the hydroxyapatite synthesized by precipitation technique formed hydroxyapatite phase slower than the hydroxyapatite synthesized by ball milling technique. The FTIR results show the chemical structures of sample in both techniques are similar. The morphology of the hydroxyapatite from the both techniques were sphere like shapes and particle size was about in nano scale. The average particle size of the hydroxyapatite by ball milling technique was less than those synthesized by precipitation technique. This experiment indicated that the ball milling technique take time less than the precipitation technique in hydroxyapatite synthesis.

Parametric evaluation of ball milling of SiC in water

NASA Technical Reports Server (NTRS)

Kiser, J. D.; Herbell, T. P.; Freedman, M. R.

1985-01-01

A statistically designed experiment was conducted to determine optimum conditions for ball milling alpha-SiC in water. The influence of pH adjustment, volume percent solids loading, and mill rotational speed on grinding effectiveness was examined. An equation defining the effect of those milling variables on specific surface area was obtained. The volume percent solids loading of the slurry had the greatest influence on the grinding effectiveness in terms of increase in specific surface area. As grinding effectiveness improved, mill and media wear also increased. Contamination was minimized by use of sintered alpha-SiC milling hardware.

Catalytically Enhanced Hydrogen Sorption in Mg-MgH2 by Coupling Vanadium-Based Catalyst and Carbon Nanotubes

PubMed Central

Kadri, Atikah; Jia, Yi; Chen, Zhigang; Yao, Xiangdong

2015-01-01

Mg (MgH2)-based composites, using carbon nanotubes (CNTs) and pre-synthesized vanadium-based complex (VCat) as the catalysts, were prepared by high-energy ball milling technique. The synergistic effect of coupling CNTs and VCat in MgH2 was observed for an ultra-fast absorption rate of 6.50 wt. % of hydrogen per minute and 6.50 wt. % of hydrogen release in 10 min at 200 °C and 300 °C, respectively. The temperature programmed desorption (TPD) results reveal that coupling VCat and CNTs reduces both peak and onset temperatures by more than 60 °C and 114 °C, respectively. In addition, the presence of both VCat and CNTs reduces the enthalpy and entropy of desorption of about 7 kJ/mol H2 and 11 J/mol H2·K, respectively, as compared to those of the commercial MgH2, which ascribe to the decrease of desorption temperature. From the study of the effect of CNTs milling time, it is shown that partially destroyed CNTs (shorter milling time) are better to enhance the hydrogen sorption performance.

Analyses of factors affecting nickel ferrite nanoparticles synthesis in ultrasound-assisted aqueous solution ball milling.

PubMed

Yuan, Zhuang; Chen, Zhen-hua; Chen, Ding; Kang, Zhi-tao

2015-01-01

Ball milling experiments were conducted with and without ultrasound wave assistance in deionized water using NiCO3·2Ni(OH)2·4H2O as raw materials. In the reaction process of NiFe2O4 prepared by ultrasound-assisted aqueous solution ball milling, some influencing factors including raw materials, ultrasonic frequency, ball to powder ratio and liquid level were changed. Samples were characterized by X-ray diffraction, fluorescence measurements and electroconductivity detections. The results indicate that more hydroxyl radicals and ions can be generated under the coupling effect of ultrasonic and ball milling. The fluorescence measurements and electroconductivity detections also reflect the reaction speed, allowing for optimal parameters to be determined. Copyright © 2014 Elsevier B.V. All rights reserved.

Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments.

PubMed

Belenguer, Ana M; Lampronti, Giulio I; Sanders, Jeremy K M

2018-01-23

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the presence of very small amounts of added solvent. To reproducibly and accurately capture this sensitivity, the experimentalist needs to carefully consider every single factor that can affect the ball mill grinding reaction under investigation, from ensuring the grinding jars are clean and dry before use, to accurately adding the stoichiometry of the starting materials, to validating that the delivery of solvent volume is accurate, to ensuring that the interaction between the solvent and the powder is well understood and, if necessary, a specific soaking time is added to the procedure. Preliminary kinetic studies are essential to determine the necessary milling time to achieve equilibrium. Only then can exquisite phase composition curves be obtained as a function of the solvent concentration under ball mill liquid assisted grinding (LAG). By using strict and careful procedures analogous to the ones here presented, such milling equilibrium curves can be obtained for virtually all milling systems. The system we use to demonstrate these procedures is a disulfide exchange reaction starting from the equimolar mixture of two homodimers to obtain at equilibrium quantitative heterodimer. The latter is formed by ball mill grinding as two different polymorphs, Form A and Form B. The ratio R = [Form B] / ([Form A] + [Form B]) at milling equilibrium depends on the nature and concentration of the solvent in the milling jar.

Scale-up of organic reactions in ball mills: process intensification with regard to energy efficiency and economy of scale.

PubMed

Stolle, Achim; Schmidt, Robert; Jacob, Katharina

2014-01-01

The scale-up of the Knoevenagel-condensation between vanillin and barbituric acid carried out in planetary ball mills is investigated from an engineering perspective. Generally, the reaction proceeded in the solid state without intermediate melting and afforded selectively only one product. The reaction has been used as a model to analyze the influence and relationship of different parameters related to operation in planetary ball mills. From the viewpoint of technological parameters the milling ball diameter, dMB, the filling degree with respect to the milling balls' packing, ΦMB,packing, and the filling degree of the substrates with respect to the void volume of the milling balls' packing, ΦGS, have been investigated at different reaction scales. It was found that milling balls with small dMB lead to higher yields within shorter reaction time, treaction, or lower rotation frequency, rpm. Thus, the lower limit is set considering the technology which is available for the separation of the milling balls from the product after the reaction. Regarding ΦMB,packing, results indicate that the optimal value is roughly 50% of the total milling beakers' volume, VB,total, independent of the reaction scale or reaction conditions. Thus, 30% of VB,total are taken by the milling balls. Increase of the initial batch sizes changes ΦGS significantly. However, within the investigated parameter range no negative influence on the yield was observed. Up to 50% of VB,total can be taken over by the substrates in addition to 30% for the total milling ball volume. Scale-up factors of 15 and 11 were realized considering the amount of substrates and the reactor volume, respectively. Beside technological parameters, variables which influence the process itself, treaction and rpm, were investigated also. Variation of those allowed to fine-tune the reaction conditions in order to maximize the yield and minimize the energy intensity.

Effects of ball milling on the physicochemical and sorptive properties of biochar: Experimental observations and governing mechanisms.

PubMed

Lyu, Honghong; Gao, Bin; He, Feng; Zimmerman, Andrew R; Ding, Cheng; Huang, Hua; Tang, Jingchun

2018-02-01

With the goal of combining the advantages of ball-milling and biochar technologies, a variety of ball-milled biochars (BM-biochars) were synthesized, characterized, and tested for nickel (Ni(II)) removal from aqueous solution. Ball milling increased only the external surface area of low temperature biochars, but still dramatically enhanced their ability to sorb aqueous Ni(II). For higher temperature biochars with relatively low surface area, ball milling increased both external and internal surface area. Measurements of pH, zeta potential, stability, and Boehm titration demonstrated that ball milling also added oxygen-containing functional groups (e.g., carboxyl, lactonic, and hydroxyl) to biochar's surface. With these changed, all the BM-biochars showed much better Ni(II) removal efficiency than unmilled biochars. Ball-milled 600 °C bagasse biochar (BMBG600) showed the greatest Ni(II) adsorption capacity (230-650 compared to 26-110 mmol/kg for unmilled biochar) and the adsorption was dosage and pH dependent. Compared with the unmilled biochar, BMBG600 also displayed faster adsorption kinetics, likely due to an increase in rates of intra-particle diffusion in the latter. Experimental and modeling results suggest that the increase in BM-biochar's external and internal surface areas exposed its graphitic structure, thus enhancing Ni(II) adsorption via strong cation-π interaction. In addition, the increase in acidic surface functional groups enhanced Ni(II) adsorption by BM-biochar via electrostatic interaction and surface complexation. Ball milling thus has great potential to increase the efficiency of environmentally friendly biochar for various environmental applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Amorphization of itraconazole by inorganic pharmaceutical excipients: comparison of excipients and processing methods.

PubMed

Grobelny, Pawel; Kazakevich, Irina; Zhang, Dan; Bogner, Robin

2015-01-01

The aim of this study was to investigate the effects of solid carriers and processing routes on the properties of amorphous solid dispersions of itraconazole. Three solid carriers with a range of surface properties were studied, (1) a mesoporous silicate, magnesium aluminum silicate (Neusilin US2), (2) a nonporous silicate of corresponding composition (Veegum) and (3) a non-silicate, inorganic excipient, calcium phosphate dibasic anhydrous (A-TAB). The drug was incorporated via either solvent-deposition or ball milling. Both the maximum drug deposited by solvent-based method that produced an amorphous composite and the time for complete amorphization by co-milling was determined by X-ray powder diffraction (XRPD). Changes in the drug and excipients were monitored by nitrogen adsorption and wettability of the powder. The ability of the excipients to amorphize the drug and enhance its dissolution was related to the powder characteristics. Neusilin provided the fastest amorphization time in the mill and highest drug loading by solvent-deposition, compared with the other two excipients. Solvent-deposition provided greater dissolution enhancement than milling, due to the reduction in Neusilin porosity during high energy milling.This study confirms that substrates as well as the processing routes have notable influence on the drug deposition, amorphization, physical stability and drug in vitro release.

Effect of Ball Mill Treatment on the Physicochemical Properties and Digestibility of Protein Extracts Generated from Scallops (Chlamys farreri)

PubMed Central

Wu, Di; Wu, Chao; Chen, Hui; Wang, Zhenyu; Yu, Cuiping; Du, Ming

2018-01-01

The effects of ball mill treatment (0, 2, 4, 6, 8, and 10 min) on the physicochemical and digestible properties of scallops (Chlamys farreri) protein (CFP) were investigated. The CFP particle size decreased with increasing ball-milling time. The content of free sulfhydryl (SH) of CFP increased from 13.08 ± 0.25 μmol/g protein to 18.85 ± 0.24 μmol/g protein when the ball-milling time increased from 0 min to 10 min. A sharp increase of the surface hydrophobicity index (H0) from 48.53 ± 0.27 to 239.59 ± 0.37 was found when the ball-milling time increased from 0 min to 4 min. Furthermore, the foaming capacity increased from 46.08 ± 6.12% to 65.11 ± 1.05% with increasing ball-milling time from 0 min to 6 min, after which it reached a plateau. SDS-PAGE results showed that ball mill treatment did not change the primary structure of CFP. Digestible properties of BMCFP simulated gastrointestinal digestion as a function of ball mill treatment were analyzed by Tricine-SDS-PAGE and nitrogen recovery index. After 60 min of simulated human gastro digestion, nitrogen recovery index of CFP had a significant rise from 42.01 ± 0.31% to 58.78 ± 3.37% as the ball-milling time increased from 0 min to 6 min. Peptides from hydrolysates of Chlamys farreri protein (CFP) were identified by ultraperformance liquidchromatographysystem coupled to a Synapt Mass Quadrupole Time-of-Flight Mass Spectrometer (UPLC-Q-TOF-MS). After 2 h and 4 h of simulated human duodenal digestion, the number of peptides with 7–10 amino acids length increased apparently with the ball-milling time increased. This study presents an approach to investigating the effect of the ball-milling process on the physicochemical and digestible properties of CFP, which may provide valuable information on the application of CFP as an ingredient in food products. PMID:29425186

Hydrogen storage materials discovery via high throughput ball milling and gas sorption.

PubMed

Li, Bin; Kaye, Steven S; Riley, Conor; Greenberg, Doron; Galang, Daniel; Bailey, Mark S

2012-06-11

The lack of a high capacity hydrogen storage material is a major barrier to the implementation of the hydrogen economy. To accelerate discovery of such materials, we have developed a high-throughput workflow for screening of hydrogen storage materials in which candidate materials are synthesized and characterized via highly parallel ball mills and volumetric gas sorption instruments, respectively. The workflow was used to identify mixed imides with significantly enhanced absorption rates relative to Li2Mg(NH)2. The most promising material, 2LiNH2:MgH2 + 5 atom % LiBH4 + 0.5 atom % La, exhibits the best balance of absorption rate, capacity, and cycle-life, absorbing >4 wt % H2 in 1 h at 120 °C after 11 absorption-desorption cycles.

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al₂O₃ Nanocomposite Synthesized by Ball Milling and Powder Metallurgy.

PubMed

Toozandehjani, Meysam; Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

2017-10-26

The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al₂O₃ (Al-5Al₂O₃) has been investigated. Al-5Al₂O₃ nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al₂O₃ nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness ( HV ), nano-hardness ( HN ), and Young's modulus ( E ) of Al-5Al₂O₃ nanocomposites. HV , HN , and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively.

Impact of initial catalyst form on the 3D structure and performance of ball-milled Ni-catalyzed MgH 2 for hydrogen storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

House, Stephen D.; Vajo, John J.; Ren, Chai

Although it has been shown that the hydrogen storage kinetics of metal hydrides can be significantly improved by the addition of transition metal-based catalysts, relatively little attention has been paid to the impact that the form in which these catalysts are introduced during synthesis has on the resulting structure and how this alters performance. Two mixtures of MgH 2 doped with Ni were prepared via high-energy ball-milling under identical conditions, one using a pure Ni nanopowder catalyst and the other using anhydrous NiCl 2. The resulting Ni catalyst particles of the NiCl 2-doped material were 10-100 times smaller, as wellmore » as more uniform in size and shape. Electron tomography revealed that the additive form also altered its incorporation and 3D spatial distribution, with Ni particles limited to the outer surface in the NiCl 2-doped case. The significantly lower desorption performance measured in the NiCl 2-doped material is attributed to regions of MgCl 2 acting as barriers between the MgH 2 and Ni, hindering the ability of the latter to effectively catalyze the reactions. Finally, this work demonstrates the hazards in assuming different catalyst forms produce similar final structures and highlights the potential of catalyst form as a synthesis tool for optimizing the material structure and performance.« less

Impact of initial catalyst form on the 3D structure and performance of ball-milled Ni-catalyzed MgH 2 for hydrogen storage

DOE PAGES

House, Stephen D.; Vajo, John J.; Ren, Chai; ...

2017-02-24

Although it has been shown that the hydrogen storage kinetics of metal hydrides can be significantly improved by the addition of transition metal-based catalysts, relatively little attention has been paid to the impact that the form in which these catalysts are introduced during synthesis has on the resulting structure and how this alters performance. Two mixtures of MgH 2 doped with Ni were prepared via high-energy ball-milling under identical conditions, one using a pure Ni nanopowder catalyst and the other using anhydrous NiCl 2. The resulting Ni catalyst particles of the NiCl 2-doped material were 10-100 times smaller, as wellmore » as more uniform in size and shape. Electron tomography revealed that the additive form also altered its incorporation and 3D spatial distribution, with Ni particles limited to the outer surface in the NiCl 2-doped case. The significantly lower desorption performance measured in the NiCl 2-doped material is attributed to regions of MgCl 2 acting as barriers between the MgH 2 and Ni, hindering the ability of the latter to effectively catalyze the reactions. Finally, this work demonstrates the hazards in assuming different catalyst forms produce similar final structures and highlights the potential of catalyst form as a synthesis tool for optimizing the material structure and performance.« less

Characterization of ball-milled carbon nanotube dispersed aluminum mixed powders

NASA Astrophysics Data System (ADS)

Maleque, M. A.; Abdullah, U.; Yaacob, I.; Ali, Y.

2016-04-01

Currently, carbon nanotube (CNT) is attracting much interest as fibrous materials for reinforcing aluminum matrix composites due to unique properties, such as high strength, elastic modulus, flexibility and high aspect ratios. However, the quality of the dispersion is the major concerning factor which determines the homogeneity of the enhanced mechanical and tribological properties of the composite. This work study and characterized carbon nanotube dispersion in ballmilled CNT-aluminum mixed powders with four different formulations such as 1, 1.5, 2 and 2.5 wt% CNT under high energy planetary ball milling operations. The ball milling was performed for two hours at constant milling speed of 250 rpm under controlled atmosphere. The characterization is performed using FESEM and EDX analyzer for mapping, elemental and line analysis. The experimental results showed homogeneous dispersion of CNTs in aluminum matrix. The composite mixture showed similar pattern from mapping, elemental and line analysis. Identification of only two peaks proved that controlled atmosphere during milling prevented the formation of inter metallic compounds such as aluminum carbide in the composite mixture. Therefore, this CNT-A1 composite powder mixture can be used for new nano-composite development without any agglomeration problem.

Synthesis and characterization of magnetite-maghemite nanoparticles obtained by the high-energy ball milling method

NASA Astrophysics Data System (ADS)

Velásquez, A. A.; Marín, C. C.; Urquijo, J. P.

2018-03-01

We present the process of synthesis and characterization of magnetite-maghemite nanoparticles by the ball milling method. The particles were synthesized in a planetary ball mill equipped with vials and balls of tempered steel, employing dry and wet conditions. For dry milling, we employed microstructured analytical-grade hematite (α-Fe2O3), while for wet milling, we mixed hematite and deionized water. Milling products were characterized by X-ray diffraction, transmission electron microscopy, room temperature Mössbauer spectroscopy, vibrating sample magnetometry, and atomic absorption spectroscopy. The Mössbauer spectrum of the dry milling product was well fitted with two sextets of hematite, while the spectrum of the wet milling product was well fitted with three sextets of spinel phase. X-ray measurements confirmed the phases identified by Mössbauer spectroscopy in both milling conditions and a reduction in the crystallinity of the dry milling product. TEM measurements showed that the products of dry milling for 100 h and wet milling for 24 h consist of aggregates of nanoparticles distributed in size, with mean particle size of 10 and 15 nm, respectively. Magnetization measurements of the wet milling product showed little coercivity and a saturation magnetization around 69 emu g-1, characteristic of a nano-spinel system. Atomic absorption measurements showed that the chromium contamination in the wet milling product is approximately two orders of magnitude greater than that found in the dry milling product for 24 h, indicating that the material of the milling bodies, liberated more widely in wet conditions, plays an important role in the conversion hematite-spinel phase.

Comparative study on the structure and electrochemical hydriding properties of MgTi, Mg 0.5Ni 0.5Ti and MgTi 0.5Ni 0.5 alloys prepared by high energy ball milling

NASA Astrophysics Data System (ADS)

Rousselot, Steeve; Guay, Daniel; Roué, Lionel

MgTi, Mg 0.5Ni 0.5Ti and MgTi 0.5Ni 0.5 alloys doped with 10 wt.% Pd were prepared by high energy ball milling and evaluated as hydrogen storage electrodes for Ni-MH batteries. X-ray diffraction analyses indicated that the Mg 0.5Ni 0.5Ti and MgTi 0.5Ni 0.5 alloys could be monophased or composed of a nanoscale mixture of MgTi + NiTi and MgTi + MgNi phases, respectively. Their hydrogen storage characteristics were investigated electrochemically in KOH electrolyte. No activation step was observed during the cycling of the Mg-Ti-Ni electrodes in contrast to that observed with the MgTi electrode. The highest hydrogen discharge capacity was obtained with the MgTi 0.5Ni 0.5 electrode (536 mAh g -1) compared to 401 and 475 mAh g -1 for the Mg 0.5Ni 0.5Ti and MgTi electrodes, respectively. The ternary Mg-Ti-Ni alloys showed a better cycle life with an average capacity decay rate per cycle lower than 1.5% compared to ∼7% for the binary MgTi electrode. The Mg-Ni-Ti electrodes also displayed a much higher discharge rate capability than the binary MgTi electrode, especially with the Mg 0.5Ni 0.5Ti electrode. The origin of this was established on the basis of the anodic polarization curves, where a substantial decrease of the concentration overpotential (reflecting a higher hydrogen diffusivity) was observed for the Mg 0.5Ni 0.5Ti electrode.

Fabrication of lanthanum-doped thorium dioxide by high-energy ball milling and spark plasma sintering

NASA Astrophysics Data System (ADS)

Scott, Spencer M.; Yao, Tiankai; Lu, Fengyuan; Xin, Guoqing; Zhu, Weiguang; Lian, Jie

2017-03-01

High-energy ball milling was used to synthesize Th1-xLaxO2-0.5x (x = 0.09, 0.23) solid solutions, as well as improve the sinterability of ThO2 powders. Dense La-doped ThO2 pellets with theoretical density above 94% were consolidated by spark plasma sintering at temperatures above 1400 °C for 20 min, and the densification behavior and the non-equilibrium effects on phase and structure were investigated. A lattice contraction of the SPS-densified pellets occurred with increasing ball milling duration, and a secondary phase with increased La-content was observed in La-doped pellets. A dependence on the La-content and sintering duration for the onset of localized phase segregation has been proposed. The effects of high-energy ball milling, La-content, and phase formation on the thermal diffusivity were also studied for La-doped ThO2 pellets by laser flash measurement. Increasing La-content and high energy ball milling time decreases thermal diffusivity; while the sintering peak temperature and holding time beyond 1600 °C dramatically altered the temperature dependence of the thermal diffusivity beyond 600 °C.

Atomic scale study of ball milled Ni-Fe{sub 2}O{sub 3} using Mössbauer spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Ravi Kumar; Govindaraj, R., E-mail: govind@igcar.gov.in; Vinod, K.

Evolution of hyperfine fields at Fe atoms has been studied in a detailed manner in a mixture of Ni and α-Fe{sub 2}O{sub 3} subjected to high energy ball milling using Mossbauer spectroscopy. Mossbauer results indicate the dispersion of α-Fe{sub 2}O{sub 3} particles in Ni matrix in the as ball milled condition. Evolution of α-Fe{sub 2}O{sub 3} due to ball milling, reduction of the valence of associated Fe and possible interaction between the oxide particles with Ni in the matrix due to annealing treatments has been elucidated in the present study.

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

PubMed

Zhang, Zhi-Yuan; Zhang, Fu-Shen; Yao, TianQi

2017-10-01

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 2 S 2 O 8 and NaCl (abbreviated as K 2 S 2 O 8 /NaCl hereafter) was the most effective co-milling reagents in terms of high recovery rate. After co-milling with K 2 S 2 O 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 0.5mol/L diluted HCl in 15min. Ag was concentrated in the leaching residue as AgCl and then recovered in 1mol/L NH 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. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis of Cu-W nanocomposite by high-energy ball milling.

PubMed

Venugopal, T; Rao, K Prasad; Murty, B S

2007-07-01

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.

Effect of ball milling on structures and properties of dispersed-type dental amalgam.

PubMed

Chern Lin, Jiin-Huey; Chen, Fred Ying-Yi; Chiang, Hui-Ju; Ju, Chien-Ping

2011-04-01

The purpose of the present study was to investigate the effect of ball milling on the initial mercury vapor release rate and mechanical properties such as compressive strength, diametral tensile strength and creep value, of the dispersed-type dental amalgam, and comparison was made with respect to two commercial amalgam alloys. Ball milling was employed to modify the configuration of the originally spherical-shaped Ag-Cu-Pd dispersant alloy particles. Improvement in mechanical properties while maintaining a low early-stage mercury vapor release rate of the amalgam is attempted. The experimental results show that the amalgam (AmB10) which was made from Ag-Cu-Pd dispersant alloy particles that were ball-milled for 10 min and heat-treated at 300 °C for 2 days exhibited a low initial mercury vapor release rate of 69 pg/mm(2)/s, which was comparable with that of commercial amalgam alloy Tytin (68 pg/mm(2)/s), and was lower than that of Dispersalloy (73 pg/mm(2)/s). As for mechanical properties, amalgam AmB10 exhibited the highest 1h compressive strength (228 MPa), which was higher than that of commercial amalgam alloy Dispersalloy by 72%; while its 24h diametral tensile strength was also the highest (177 MPa), and was higher than that of Dispersalloy by 55%. Furthermore, the creep value of the amalgams made from Ag-Cu-Pd alloy particles with 10 min ball-milling and heat treatment at 300 °C for 2 days was measured to be 0.12%, which was about 20% that of Dispersalloy. It is found that ball milling of the dispersant Ag-Cu-Pd alloy particles for 10 min was able to modify the configuration of the alloy particles into irregular-shapes. Subsequently, heat treatment at 300 °C significantly lowered the initial mercury vapor release rate, increased its 1h compressive strength and 1h diametral tensile strength, and lowered its creep value. Copyright © 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

One step conversion of wheat straw to sugars by simultaneous ball milling, mild acid, and fungus Penicillium simplicissimum treatment.

PubMed

Yuan, Li; Chen, Zhenhua; Zhu, Yonghua; Liu, Xuanming; Liao, Hongdong; Chen, Ding

2012-05-01

Wheat straw is one of the major lignocellulosic plant residues in many countries including China. An attractive alternative is the utilization of wheat straw for bioethanol production. This article mainly studies a simple one-step wet milling with Penicillium simplicissimum and weak acid to hydrolysis of wheat straw. The optimal condition for hydrolysis was ball milling 48 h in citrate solvent (pH = 4) with P. simplicissimum H5 at the speed of 500 rpm and the yield of sugar increased with increased milling time. Corresponding structure transformations before and after milling analyzed by X-ray diffraction, transmission Fourier transform infrared spectroscopy, and environmental scanning electron microscopy clearly indicated that this combined treatment could be attributed to the crystalline and chemical structure changes of cellulose in wheat straw during ball milling. This combined treatment of ball milling, mild acid, and fungus hydrolysis enabled the conversion of the wheat straw. Compared with traditional method of ball milling, this work showed a more simple, novel, and environmentally friendly way in mechanochemical treatment of wheat straw.

Magnetoresistivity and microstructure of YBa2Cu3Oy prepared using planetary ball milling

NASA Astrophysics Data System (ADS)

Hamrita, A.; Ben Azzouz, F.; Madani, A.; Ben Salem, M.

2012-01-01

We have studied the microstructure and the magnetoresistivity of polycrystalline YBa2Cu3Oy (YBCO or Y-123 for brevity) embedded with nanoparticles of Y-deficient YBCO, generated by the planetary ball milling technique. Bulk samples were synthesized from a precursor YBCO powder, which was prepared from commercial high purity Y2O3, Ba2CO3 and CuO via a one-step annealing process in air at 950 °C. After planetary ball milling of the precursor, the powder was uniaxially pressed and subsequently annealed at 950 °C in air. Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM), microstructure investigation by transmission electron microscopy (TEM) coupled with energy dispersive X-ray spectroscopy (EDXS) were carried out. TEM analyses show that nanoparticles of Y-deficient YBCO, generated by ball milling, are embedded in the superconducting matrix. Electrical resistance as a function of temperature, ρ(T), revealed that the zero resistance temperature, Tco, is 84.5 and 90 K for the milled and unmilled samples respectively. The milled ceramics exhibit a large magnetoresistance in weak magnetic fields at liquid nitrogen temperature. This attractive effect is of high significance as it makes these materials promising candidates for practical application in magnetic field sensor devices.

Effect of ball-milling surfactants on the interface chemistry in hot-compacted SmCo5 magnets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, WF; Sepehri-Amin, H; Zheng, LY

2012-11-01

Anisotropic SmCo5 nanoflakes prepared by high-energy ball-milling with surfactants have great potential in applications for high-performance nanocomposite magnets. For such "nanocomposite" applications, the surface structure and chemistry of nanoflakes are crucial for achieving high coercivity. In this study, hot-pressed samples from anisotropic SmCo5 nanoflakes, ball-milled with different surfactants, oleic acid (OA) and oleylamine (OY), were investigated. Interface layers between the SmCo5 nanoflakes were found to consist of samarium oxides and a soft magnetic Co phase. These surface layers contribute to the degradation of hard magnetic performance, which is confirmed by scanning transmission electron microscopy-energy dispersive X-ray spectroscopy analysis of themore » cross-section of a single flake ball-milled with OA. Samples milled with OY show a much thinner interface layer in compacted samples, which means that the surface degradation during ball-milling with OY is much less than that with OA. The results show clearly that the choice of proper surfactant and the control of processing parameters are the key factors for improving the surface condition of the nanoflakes and the resulting hard magnetic properties. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.« less

Amorphization induced by focused ion beam milling in metallic and electronic materials.

PubMed

Huh, Yoon; Hong, Ki Jung; Shin, Kwang Soo

2013-08-01

Focused ion beam (FIB) milling using high-energy gallium ions is widely used in the preparation of specimens for transmission electron microscopy (TEM). However, the energetic ion beam induces amorphization on the edge of specimens during milling, resulting in a mischievous influence on the clearness of high-quality transmission electron micrographs. In this work, the amorphization induced by the FIB milling was investigated by TEM for three kinds of materials, metallic materials in bulk shape, and semiconductive and electronic ceramic materials as a substrate for the deposition of thin films.

Effect of amorphous lamella on the crack propagation behavior of crystalline Mg/amorphous Mg-Al nanocomposites

NASA Astrophysics Data System (ADS)

Hai-Yang, Song; Yu-Long, Li

2016-02-01

The effects of amorphous lamella on the crack propagation behavior in crystalline/amorphous (C/A) Mg/Mg-Al nanocomposites under tensile loading are investigated using the molecular dynamics simulation method. The sample with an initial crack of orientation [0001] is considered here. For the nano-monocrystal Mg, the crack growth exhibits brittle cleavage. However, for the C/A Mg/Mg-Al nanocomposites, the ‘double hump’ behavior can be observed in all the stress-strain curves regardless of the amorphous lamella thickness. The results indicate that the amorphous lamella plays a critical role in the crack deformation, and it can effectively resist the crack propagation. The above mentioned crack deformation behaviors are also disclosed and analyzed in the present work. The results here provide a strategy for designing the high-performance hexagonal-close-packed metal and alloy materials. Project supported by the National Natural Science Foundation of China (Grant Nos. 11372256 and 11572259), the 111 Project (Grant No. B07050), the Program for New Century Excellent Talents in University of Ministry of Education of China (Grant No. NCET-12-1046), and the Program for New Scientific and Technological Star of Shaanxi Province, China (Grant No. 2012KJXX-39).

Considerations on the quantitative analysis of apparent amorphicity of milled lactose by Raman spectroscopy.

PubMed

Pazesh, Samaneh; Lazorova, Lucia; Berggren, Jonas; Alderborn, Göran; Gråsjö, Johan

2016-09-10

The main purpose of the study was to evaluate various pre-processing and quantification approaches of Raman spectrum to quantify low level of amorphous content in milled lactose powder. To improve the quantification analysis, several spectral pre-processing methods were used to adjust background effects. The effects of spectral noise on the variation of determined amorphous content were also investigated theoretically by propagation of error analysis and were compared to the experimentally obtained values. Additionally, the applicability of calibration method with crystalline or amorphous domains in the estimation of amorphous content in milled lactose powder was discussed. Two straight baseline pre-processing methods gave the best and almost equal performance. By the succeeding quantification methods, PCA performed best, although the classical least square analysis (CLS) gave comparable results, while peak parameter analysis displayed to be inferior. The standard deviations of experimental determined percentage amorphous content were 0.94% and 0.25% for pure crystalline and pure amorphous samples respectively, which was very close to the standard deviation values from propagated spectral noise. The reasonable conformity between the milled samples spectra and synthesized spectra indicated representativeness of physical mixtures with crystalline or amorphous domains in the estimation of apparent amorphous content in milled lactose. Copyright © 2016 The Author(s). Published by Elsevier B.V. All rights reserved.

Design and Testing of UMM Vertical Ball Mill (UVBM) for producing Aluminium Powder

NASA Astrophysics Data System (ADS)

Aisyah, I. S.; Caesarendra, Wahyu; Suprihanto, Agus

2018-04-01

UMM Vertical Ball Mill (UVBM) was intended to be the apparatus to produce metal powder with superior characteristic in production rate while retaining good quality of metal powder. The concept of design was adopting design theory of Phal and Beitz with emphasis on increasing of probability of success in engineering and economy aspects.Since it was designed as vertical ball mill, a new way to produce powder, then it need to be tested for the performance after manufactured. The test on UVBM was carried out by milling of aluminium chip for 5 (five) different milling time of 0.5 hours, 1 hour, 3 hours, 5 hours and 7 hours, and the powder product then be characterized for it morphology and size using Scanning Electron Microscope (SEM) and Sieve.The results of the study were the longer of the milling time, the finer of the powder. From the test results of SEM, the morphology of the powder with 5 variations of milling time were most of the powder in form of flake (flat), small round and angular (irregular). The distribution of powder size was best obtained on the variation of milling time 3 hours, 5 hours, and 7 hours with percentage of 200 mesh in size of 22.14 %, 64 % and 91.25 % respectively.

Contamination risk of stable isotope samples during milling.

PubMed

Isaac-Renton, M; Schneider, L; Treydte, K

2016-07-15

Isotope analysis of wood is an important tool in dendrochronology and ecophysiology. Prior to mass spectrometry analysis, wood must be homogenized, and a convenient method involves a ball mill capable of milling samples directly in sample tubes. However, sample-tube plastic can contaminate wood during milling, which could lead to biological misinterpretations. We tested possible contamination of whole wood and cellulose samples during ball-mill homogenization for carbon and oxygen isotope measurements. We used a multi-factorial design with two/three steel milling balls, two sample amounts (10 mg, 40 mg), and two milling times (5 min, 10 min). We further analyzed abrasion by milling empty tubes, and measured the isotope ratios of pure contaminants. A strong risk exists for carbon isotope bias through plastic contamination: the δ(13) C value of polypropylene deviated from the control by -6.77‰. Small fibers from PTFE filter bags used during cellulose extraction also present a risk as the δ(13) C value of this plastic deviated by -5.02‰. Low sample amounts (10 mg) showed highest contamination due to increased abrasion during milling (-1.34‰), which is further concentrated by cellulose extraction (-3.38‰). Oxygen isotope measurements were unaffected. A ball mill can be used to homogenize samples within test tubes prior to oxygen isotope analysis, but not prior to carbon or radiocarbon isotope analysis. There is still a need for a fast, simple and contamination-free sample preparation procedure. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

PubMed Central

Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

2017-01-01

The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3) has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV), nano-hardness (HN), and Young’s modulus (E) of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively. PMID:29072632

Production of pyrite nanoparticles using high energy planetary ball milling for sonocatalytic degradation of sulfasalazine.

PubMed

Khataee, Alireza; Fathinia, Siavash; Fathinia, Mehrangiz

2017-01-01

Sonocatalytic performance of pyrite nanoparticles was evaluated by the degradation of sulfasalazine (SSZ). Pyrite nanoparticles were produced via a high energy mechanical ball milling (MBM) in different processing time from 2h to 6h, in the constant milling speed of 320rpm. X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR) analysis and Brunauer-Emmett-Teller (BET) confirmed the production of pyrite nanoparticles during 6h of ball milling with the average size distribution of 20-80nm. The effects of various operational parameters including pH value, catalyst amount (mg/L), SSZ concentration (mg/L), ultrasonic frequency (kHz) and reaction time on the SSZ removal efficiency were examined. The obtained results showed that the maximum removal efficiency of 97.00% was obtained at pH value of 4, catalyst dosage of 0.5g/L, SSZ concentration of 10mg/L and reaction time of 30min. Experimental results demonstrated that the kinetic of the degradation process can be demonstrated using Langmuir-Hinshelwood (L-H) kinetic model. The effect of different inorganic ions such as Cl - , CO 3 2- and SO 4 2- was investigated on the L-H reaction rate (k r ) and adsorption (K s ) constants. Results showed that the presence of the mentioned ions significantly influenced the L-H constants. The impact of ethanol as a OH radical scavenger and some enhancers including H 2 O 2 and K 2 S 2 O 8 was investigated on the SSZ removal efficiency. Accordingly, the presence of ethanol suppressed SSZ degradation due to the quenching of OH radicals and the addition of K 2 S 2 O 8 and H 2 O 2 increased the SSZ removal efficiency, due to the formation of SO 4 - and additional OH radicals, respectively. Under the identical conditions of operating parameters, pyrite nanoparticles maintained their catalytic activity during four consecutive runs. Copyright © 2016 Elsevier B.V. All rights reserved.

6. FF coal pulverizer (ball mill inside). GG building in ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. FF coal pulverizer (ball mill inside). GG building in background did preliminary crushing; pulverizer to left, coal conveyor and air cleaning towers to right; conveyor on left brought crushed coal to FF. Looking north/northeast - Rouge Steel Company, 3001 Miller Road, Dearborn, MI

Heterogeneous sono-Fenton-like process using martite nanocatalyst prepared by high energy planetary ball milling for treatment of a textile dye.

PubMed

Dindarsafa, Mahsa; Khataee, Alireza; Kaymak, Baris; Vahid, Behrouz; Karimi, Atefeh; Rahmani, Amir

2017-01-01

High energy planetary ball milling was applied to prepare sono-Fenton nanocatalyst from natural martite (NM). The NM samples were milled for 2-6h at the speed of 320rpm for production of various ball milled martite (BMM) samples. The catalytic performance of the BMMs was greater than the NM for treatment of Acid Blue 92 (AB92) in heterogeneous sono-Fenton-like process. The NM and the BMM samples were characterized by XRD, FT-IR, SEM, EDX and BET analyses. The particle size distribution of the 6h-milled martite (BMM 3 ) was in the range of 10-90nm, which had the highest surface area compared to the other samples. Then, the impact of main operational parameters was investigated on the process. Complete removal of the dye was obtained at the desired conditions including initial pH 7, 2.5g/L BMM 3 dosage, 10mg/L AB92 concentration, and 150W ultrasonic power after 30min of treatment. The treatment process followed pseudo-first order kinetic. Environmentally-friendly modification of the NM, low leached iron amount and repeated application at milder pH were the significant benefits of the BMM 3 . The GC-MS was successfully used to identify the generated intermediates. Eventually, an artificial neural network (ANN) was applied to predict the AB92 removal efficiency based upon the experimental data with a proper correlation coefficient (R 2 =0.9836). Copyright © 2016 Elsevier B.V. All rights reserved.

Long-Term Effects on Graphene Supercapacitors of Using a Zirconia Bowl and Zirconia Balls for Ball-Mill mixing of Active Materials

NASA Astrophysics Data System (ADS)

Song, Dae-Hoon; Kim, Jin-Young; Kahng, Yung Ho; Cho, Hoonsung; Kim, Eung-Sam

2018-04-01

Improving the energy storage performance of supercapacitor electrodes based on reduced graphene oxide (RGO) is one of the main subjects in this research field. However, when a zirconia bowl and zirconia balls were used for ball-mill mixing of the active materials for RGO supercapacitors, the energy storage performance deteriorated over time. Our study revealed that the source of the problem was the inclusion of zirconia bits from abrasion of the bowl and the balls during the ballmill mixing, which increased during a period of 1 year. We probed two solutions to this problem: 1) hydrofluoric (HF) acid treatment of the RGO supercapacitors and 2) use of a tempered steel bowl and tempered steel balls for the mixing. For both cases, the energy storage performance was restored to near the initial level, showing a specific capacitance ( C sp ) of 200 F/g. Our results should lead to progress in research on RGO supercapacitors.

Excess lithium storage in LiFePO4-Carbon interface by ball-milling

NASA Astrophysics Data System (ADS)

Guo, Hua; Song, Xiaohe; Zheng, Jiaxin; Pan, Feng

2016-07-01

As one of the most popular cathode materials for high power lithium ion batteries (LIBs) of the electrical-vehicle (EV), lithium iron phosphate (LiFePO4 (LFP)) is limited to its relatively lower theoretical specific capacity of 170mAh g-1. To break the limits and further improve the capacity of LFP is promising but challenging. In this study, the ball-milling method is applied to the mixture of LFP and carbon, and the effective capacity larger than the theoretical one by 30mAh g-1 is achieved. It is demonstrated that ball-milling leads to the LFP-Carbon interface to store the excess Li-ions.

A Reaction-ball-milling-driven Surface Coating Strategy to Suppress Pulverization of Microparticle Si Anodes.

PubMed

Yang, Yaxiong; Qu, Xiaolei; Zhang, Lingchao; Gao, Mingxia; Liu, Yongfeng; Pan, Hongge

2018-06-01

In this work, we report on a novel reaction-ball-milling surface coating strategy to suppress the pulverization of microparticle Si anodes upon lithiation/delithiation. By energetic milling the partially prelithiated microparticle Si in a CO2 atmosphere, a multicomponent amorphous layer composed of SiOx, C, SiC and Li2SiO3 is successfully coated on the surface of Si microparticles. The coating level strongly depends on the milling reaction duration, and the 12-h milled prelithiated Si microparticles (BM12h) under a pressure of 3 bar of CO2 exhibits a good conformal coating with 1.006 g cm3 of tap density. The presence of SiC remarkably enhances the mechanical properties of the SiOx/C coating matrix with an approximately 4-fold increase in the elastic modulus and the hardness values, which effectively alleviates the global volume expansion of the Si microparticles upon lithiation. Simultaneously, the existence of Li2SiO3 insures the Li-ion conductivity of the coating layer. Moreover, the SEI film formed on the electrode surface maintains relatively stable upon cycling due to the remarkably suppressed crack and pulverization of particles. These processes work together to allow the BM12h sample to offer much better cycling stability, as its reversible capacity remains at 1439 mAh g-1 at 100 mA g-1 after 100 cycles, which is nearly 4 times that of the pristine Si microparticles (381 mAh g-1). This work opens up new opportunities for the practical applications of micrometre-scaled Si anode.

Influence of ball milling on the particle size and antimicrobial properties of Tridax procumbens leaf nanoparticles.

PubMed

Karthik, Subramani; Suriyaprabha, Rangaraj; Balu, Kolathupalayam Shanmugam; Manivasakan, Palanisamy; Rajendran, Venkatachalam

2017-02-01

The herbal nanoparticles were prepared from shade dried Tridax procumbens plant leaves employing ball milling technique using different process parameters, like ball ratio/size and milling time. The obtained nanoparticles were comprehensively characterised using X-ray diffraction, Fourier transform infrared spectroscopy, UV-visible spectroscopy, dynamic light scattering, scanning electron microscopy and antimicrobial analysis techniques. The crystallinity of the nanoparticles was retained without altering even though the particle size changes due to milling periods. The antibacterial activities of the prepared herbal nanoparticles against Staphylococcus aureus and Escherichia coli were explored to understand the influence of particle size on antimicrobial activities and their functional properties. The increase in ball ratio and milling time periods leads to a decrease in nanoparticle size from 114 to 45 nm which in turn increases the antimicrobial activities. The above study confirms that antimicrobial activity relies on nanoparticle size. The observed knowledge on influence of particle size on antimicrobial activities will help to optimise the production of potential herbal nanoparticles for different biomedical applications.

ZnO nanoparticles obtained by ball milling technique: Structural, micro-structure, optical and photo-catalytic properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balamurugan, S., E-mail: scandium.chemistry@gmail.com; Joy, Josny; Godwin, M. Anto

The ZnO nanoparticles were obtained by ball milling of commercial grade ZnO powder at 250 rpm for 20 h and studied their structural, micro-structure, optical and photo-catalytic properties. Due to ball milling significant decrease in lattice parameters and average crystalline size is noticed for the as-milled ZnO nano powder. The HRSEM images of the as-milled powder consist of agglomerated fine spherical nanoparticles in the range of ~10-20 nm. The room temperature PL spectrum of as-milled ZnO nano powder excited under 320 nm reveals two emission bands at ~406 nm (violet emission) and ~639 nm (green emission). Interestingly about 98 % of photo degradation of methylene (MB)more » by the ZnO catalyst is achieved at 100 minutes of solar light irradiation.« less

Characterization of melt-quenched and milled amorphous solids of gatifloxacin.

PubMed

Hattori, Yusuke; Suzuki, Ayumi; Otsuka, Makoto

2016-11-01

The objectives of this study were to characterize and investigate the differences in amorphous states of gatifloxacin. We prepared two types of gatifloxacin amorphous solids coded as M and MQ using milling and melt-quenching methods, respectively. The amorphous solids were characterized via X-ray diffraction (XRD), nonisothermal differential scanning calorimetry (DSC) and time-resolved near-infrared (NIR) spectroscopy. Both the solids displayed halo XRD patterns, the characteristic of amorphous solids; however, in the non-isothermal DSC profiles, these amorphous solids were distinguished by their crystallization and melting temperatures. The Kissinger-Akahira-Sunose plots of non-isothermal crystallization temperatures at various heating rates indicated a lower activation energy of crystallization for the amorphous solid M than that of MQ. These results support the differentiation between two amorphous states with different physical and chemical properties.

Microstructure and Mechanical Behavior of Microwave Sintered Cu50Ti50 Amorphous Alloy Reinforced Al Metal Matrix Composites

NASA Astrophysics Data System (ADS)

Reddy, M. Penchal; Ubaid, F.; Shakoor, R. A.; Mohamed, A. M. A.

2018-06-01

In the present work, Al metal matrix composites reinforced with Cu-based (Cu50Ti50) amorphous alloy particles synthesized by ball milling followed by a microwave sintering process were studied. The amorphous powders of Cu50Ti50 produced by ball milling were used to reinforce the aluminum matrix. They were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and compression testing. The analysis of XRD patterns of the samples containing 5 vol.%, 10 vol.% and 15 vol.% Cu50Ti50 indicates the presence of Al and Cu50Ti50 peaks. SEM images of the sintered composites show the uniform distribution of reinforced particles within the matrix. Mechanical properties of the composites were found to increase with an increasing volume fraction of Cu50Ti50 reinforcement particles. The hardness and compressive strength were enhanced to 89 Hv and 449 MPa, respectively, for the Al-15 vol.% Cu50Ti50 composites.

Synthesis of Nano-Size AlN Powders by Carbothermal Reduction from Plasma-Assisted Ball Milling Precursor

NASA Astrophysics Data System (ADS)

Liu, Zhijie; Wang, Wenchun; Yang, Dezheng; Wang, Sen; Dai, Leyang

2016-07-01

Nano-size aluminum nitride (AlN) powders have been successfully synthesized with a high efficiency method through annealing from milling assisted by discharge plasma (p-milling) alumina (Al2O3) precursors. The characterization of the p-milling Al2O3 powders and the synthesized AlN are investigated. Compared to conventional ball milling (c-milling), it can be found that the precursors by p-milling have a finer grain size with a higher specific surface area, which lead to a faster reaction efficiency and higher conversion to AlN at lower temperatures. The activation energy of p-milling Al2O3 is found to be 371.5 kJ/mol, a value that is much less than the reported value of the unmilled and the conventional milled Al2O3. Meanwhile, the synthesized AlN powders have unique features, such as an irregular lamp-like morphology with uniform particle distribution and fine average particle size. The results are attributed to the unique synergistic effect of p-milling, which is the effect of deformation, fracture, and cold welding of Al2O3 powders resulting from ball milling, that will be enhanced due to the introduction of discharge plasma. supported by National Natural Science Foundation of China (No. 51177008)

Atomic simulations of deformation mechanisms of crystalline Mg/amorphous Mg-Al nanocomposites

NASA Astrophysics Data System (ADS)

Song, H. Y.; Li, Y. L.

2015-09-01

The effects of amorphous boundary (AB) spacing on the deformation behavior of crystalline/amorphous (C/A) Mg/Mgsbnd Al nanocomposites under tensile load are investigated using molecular dynamics method. The results show that the plasticity of nano-polycrystal Mg can be enhanced with the introduction of C/A interfaces. For samples 5.2 nm in AB spacing and larger, the superior tensile ductility and nearly perfect plastic flow behavior occur during plastic deformation. The studies indicate that the cooperative interactions between crystalline and amorphous are the main reason for excellent ductility enhancements in C/A Mg/Mgsbnd Al nanocomposites.

Influence of milling time on fineness of Centella Asiatica particle size produced using planetary ball mill

NASA Astrophysics Data System (ADS)

Borhan, M. Z.; Ahmad, R.; Rusop, M.; Abdullah, S.

2012-11-01

Centella Asiatica (C. Asiatica)contains asiaticoside as bioactive constituent which can be potentially used in skin healing process. Unfortunately, the normal powders are difficult to be absorbed by the body effectively. In order to improve the value of use, nano C. Asiatica powder was prepared. The influence of milling time was carried out at 0.5, 2, 4, 6, 8 hours and 10 hours. The effect of ball milling at different times was characterized using particles size analysis and FTIR Spectroscopy. The fineness of ground product was evaluated by recording the z-Average (nm), undersize distribution and polydispersity index (PdI). The results show that the smallest size particles by mean is 233 nm while FTIR spectra shows that there is no changing in the major component in the C. Asiatica powders with milling time.

Influence of in situ and ex situ ZrO2 addition on the properties of MgB2

NASA Astrophysics Data System (ADS)

Chen, S. K.; Glowacki, B. A.; MacManus-Driscoll, J. L.; Vickers, M. E.; Majoros, M.

2004-02-01

The effect of ZrO2 addition on the properties of MgB2 has been studied using in situ and ex situ processes. The in situ process was performed by introducing ZrO2 from the milling tools into MgB2 throughout the planetary ball milling, whereas the ex situ process was accomplished by mixing ZrO2 from the milling tools with MgB2 by hand grinding in a mortar. A detectable amount of ZrO2 was present in MgB2 after 4 h of milling during the in situ process and its content increased with milling time as expected. The 400 h milled powder was partially amorphized and showed the formation of a minority ZrB2 phase. For milling up to 100 h, diamagnetism of MgB2 was significantly reduced while Tc remained unchanged. Superconductivity was totally destroyed after 148 h of milling. The loss of superconductivity is attributed to the effect of disordering induced by mechanical milling. As a result of in situ ZrO2 addition, the initial Tc and crystal structure of MgB2 could not be restored upon annealing. With increasing milling time, the expansion of lattice parameters in both the a-axis and c-axis may be due to possible substitution of Mg or B by Zr. The result from the magnetic measurement shows that Jc of MgB2 is deteriorated by in situ ZrO2 addition. On the other hand, ex situ ZrO2 addition with annealing did not degrade the Tc of MgB2.

Study of the preparation of Cu-TiC composites by reaction of soluble Ti and ball-milled carbon coating TiC

NASA Astrophysics Data System (ADS)

Xu, Xuexia; Li, Wenbin; Wang, Yong; Dong, Guozhen; Jing, Shangqian; Wang, Qing; Feng, Yanting; Fan, Xiaoliang; Ding, Haimin

2018-06-01

In this work, Cu-TiC composites have been successfully prepared by reaction of soluble Ti and carbon coating TiC. Firstly, the ball milling of graphite and TiC mixtures is used to obtain the carbon coating TiC which has fine size and improved reaction activity. After adding the ball milled carbon coating TiC into Cu-Ti melts, the soluble Ti will easily react with the carbon coating to form TiC. This process will also improve the wettability between Cu melts and TiC core. As a result, besides the TiC prepared by reaction of soluble Ti and carbon coating, the ball milled TiC will also be brought into the melts. Some of these ball-milled TiC particles will go on being coated by the formed TiC from the reaction of Ti and the coating carbon and left behind in the composites. However, most of TiC core will be further reacted with the excessive Ti and be transformed into the newly formed TiC with different stoichiometry. The results indicate that it is a feasible method to synthesize TiC in Cu melts by reaction of soluble Ti and ball-milled carbon coating TiC.

Amorphous GeOx-Coated Reduced Graphene Oxide Balls with Sandwich Structure for Long-Life Lithium-Ion Batteries.

PubMed

Choi, Seung Ho; Jung, Kyeong Youl; Kang, Yun Chan

2015-07-01

Amorphous GeOx-coated reduced graphene oxide (rGO) balls with sandwich structure are prepared via a spray-pyrolysis process using polystyrene (PS) nanobeads as sacrificial templates. This sandwich structure is formed by uniformly coating the exterior and interior of few-layer rGO with amorphous GeOx layers. X-ray photoelectron spectroscopy analysis reveals a Ge:O stoichiometry ratio of 1:1.7. The amorphous GeOx-coated rGO balls with sandwich structure have low charge-transfer resistance and fast Li(+)-ion diffusion rate. For example, at a current density of 2 A g(-1), the GeOx-coated rGO balls with sandwich and filled structures and the commercial GeO2 powders exhibit initial charge capacities of 795, 651, and 634 mA h g(-1), respectively; the corresponding 700th-cycle charge capacities are 758, 579, and 361 mA h g(-1). In addition, at a current density of 5 A g(-1), the rGO balls with sandwich structure have a 1600th-cycle reversible charge capacity of 629 mA h g(-1) and a corresponding capacity retention of 90.7%, as measured from the maximum reversible capacity at the 100th cycle.

Germanium and Tin Based Anode Materials for Lithium-Ion Batteries

NASA Astrophysics Data System (ADS)

Ji, Dongsheng

The discovery of safe anode materials with high energy density for lithium-ion batteries has always been a significant topic. Group IV elements have been under intensive study for their high capability of alloying with lithium. Batteries with graphite and tin based anode material have already been applied in cell phones and vehicles. In order to apply group IV elements, their dramatic volume change during lithiation and delithiation processes is the key point to work on. Reducing the particle size is the most common method to buffer the volume expansion. This strategy has been applied on both germanium and tin based materials. Germanium based anode material has been made by two different synthesis methods. The amorphous Ge-C-Ti composite material was made by ball milling method and performed much better than other germanium alloy including Ge-Mg, Ge-Fe and Ge-Fe.Germanium sphere nano particles with diameter of around 50 nm have been made by solution method. After ball milled with graphite, the resulted product performed stable capacity over 500 mAh˙g-1 for more than 20 cycles. Ball milled graphite in the composite plays an important role of buffering volume change and stabilizing germanium. Sn-Fe alloy is one of the feasible solutions to stabilize tin. Sn 2Fe-C composite has been made by ball milling method. After optimizations of the ratio of precursors, reaction time, milling balls and electrolyte additives, the electrochemistry performance was improved. The anode performed 420 mAh˙ -1 at 1.0 mA/cm2 and maintained its structure after cycling at 2.0 mA/cm2. At 0.3 mA/cm2 cycling rate, the anode performed 978 mAh/cm3 after 500 cycles, which still exceeds the theoretical capacity of graphite.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bajorek, Anna, E-mail: anna.bajorek@us.edu.pl; Silesian Center for Education and Interdisciplinary Research, University of Silesia, 75 Pułku Piechoty 1A, 41-500 Chorzów; Skornia, Paweł

2015-03-15

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. Themore » 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.« less

Mechanical intermixing of components in (CoMoNi)-based systems and the formation of (CoMoNi)/WC nanocomposite layers on Ti sheets under ball collisions

NASA Astrophysics Data System (ADS)

Romankov, S.; Park, Y. C.; Shchetinin, I. V.

2017-11-01

Cobalt (Co), molybdenum (Mo), and nickel (Ni) components were simultaneously introduced onto titanium (Ti) surfaces from a composed target using ball collisions. Tungsten carbide (WC) balls were selected for processing as the source of a cemented carbide reinforcement phase. During processing, ball collisions continuously introduced components from the target and the grinding media onto the Ti surface and induced mechanical intermixing of the elements, resulting in formation of a complex nanocomposite structure onto the Ti surface. The as-fabricated microstructure consisted of uniformly dispersed WC particles embedded within an integrated metallic matrix composed of an amorphous phase with nanocrystalline grains. The phase composition of the alloyed layers, atomic reactions, and the matrix grain sizes depended on the combination of components introduced onto the Ti surface during milling. The as-fabricated layer exhibited a very high hardness compared to industrial metallic alloys and tool steel materials. This approach could be used for the manufacture of both cemented carbides and amorphous matrix composite layers.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

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 themore » 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.« less

Impact of planetary ball milling parameters on the microstructure and pinning properties of polycrystalline superconductor Y3Ba5Cu8Oy

NASA Astrophysics Data System (ADS)

Slimani, Y.; Hannachi, E.; Azzouz, F. Ben; Salem, M. Ben

2018-06-01

We have reported the influence of planetary high energy ball milling parameters on morphology, microstructure and flux pinning capability of polycrystalline Y3Ba5Cu8Oy. Samples were prepared through the standard solid-state reaction by using two different milling methods, ball milling in a planetary crusher and hand grinding in a mortar. Phase analysis by X-ray diffraction (XRD) method, microstructural examination by scanning electron microscope (SEM), electrical resistivity, the global and intra-granular critical current densities measurements are done to characterize the samples. The processing parameters of the planetary milling have a considerable impact on the final product properties. SEM observations show the presence of nanoscale entities submerged within the Y3Ba5Cu8Oy crystallites. The results show that the fine grain microstructure of the Y3Ba5Cu8Oy bulk induced by ball milling process contributes to critical currents density enhancement in the magnetic field and promotes an optimized flux pinning ability.

Crystallization Behavior of A Bulk Amorphous Mg62Cu26Y12 Alloy

NASA Astrophysics Data System (ADS)

Wu, Shyue-Sheng; Chin, Tsung-Shune; Su, Kuo-Chang

1994-07-01

The crystallization temperature, the associated activation energy and the crystallized structure of a bulk amorphous Mg62Cu26Y12 alloy with a diameter of 2.5 mm were studied. It possesses a one-step crystallization behavior. The crystallization reaction was found to be represented by: AM(MG62Cu26Y12)→Mg2Cu+MgY+CuY+Mg, ( Tx=188°C, Eac=134 kJ/mol) where AM represents the amorphous state, T x the crystallization temperature at an infinitesimal heating rate, and E ac the associated activation energy. The amount of crystalline phases were found to be Mg2Cu:MgY:CuY=76:17:7. The Mg phase is identifiable only by high resolution electron microscopy, not by X-ray diffraction. The crystallization leads to a sharp rise in electrical resistivity which is reversed to those of iron-based amorphous alloys.

Application of a Salt Coformer in a Co-Amorphous Drug System Dramatically Enhances the Glass Transition Temperature: A Case Study of the Ternary System Carbamazepine, Citric Acid, and l-Arginine.

PubMed

Ueda, Hiroshi; Wu, Wenqi; Löbmann, Korbinian; Grohganz, Holger; Müllertz, Anette; Rades, Thomas

2018-05-07

The use of co-amorphous systems containing a combination of low molecular weight drugs and excipients is a relatively new technology in the pharmaceutical field to improve the solubility of poorly water-soluble drugs. However, some co-amorphous systems show a lower glass transition temperature ( T g ) than many of their polymeric solid dispersion counterparts. In this study, we aimed at designing a stable co-amorphous system with an elevated T g . Carbamazepine (CBM) and citric acid (CA) were employed as the model drug and the coformer, respectively. co-amorphous CBM-CA at a 1:1 molar ratio was formed by ball milling, but a transition from the glassy to the supercooled melt state was observed under ambient conditions, due to the relatively low T g of 38.8 °C of the co-amorphous system and moisture absorption. To improve the T g of the coformer, salt formation of a combination of l-arginine (ARG) with CA was studied. First, ball milling of CA-ARG at molar ratios of 1:1, 1:2, and 1:3 forming co-amorphous systems was performed and led to a dramatic enhancement of the T g , depending on the CA-ARG ratio. Salt formation between CA and ARG was observed by infrared spectroscopy. Next, ball milling of CBM-CA-ARG at molar ratios of 1:1:1, 1:1:2, and 1:1:3 resulted in co-amorphous blends, which had a single T g at 77.8, 105.3, and 127.8 °C, respectively. These ternary co-amorphous samples remained in a solid amorphous form for 2 months at 40 °C. From these results, it can be concluded that blending of the salt coformer with a drug is a promising strategy to design stable co-amorphous formulations.

Bioethanol production from ball milled bagasse using an on-site produced fungal enzyme cocktail and xylose-fermenting Pichia stipitis.

PubMed

Buaban, Benchaporn; Inoue, Hiroyuki; Yano, Shinichi; Tanapongpipat, Sutipa; Ruanglek, Vasimon; Champreda, Verawat; Pichyangkura, Rath; Rengpipat, Sirirat; Eurwilaichitr, Lily

2010-07-01

Sugarcane bagasse is one of the most promising agricultural by-products for conversion to biofuels. Here, ethanol fermentation from bagasse has been achieved using an integrated process combining mechanical pretreatment by ball milling, with enzymatic hydrolysis and fermentation. Ball milling for 2 h was sufficient for nearly complete cellulose structural transformation to an accessible amorphous form. The pretreated cellulosic residues were hydrolyzed by a crude enzyme preparation from Penicillium chrysogenum BCC4504 containing cellulase activity combined with Aspergillus flavus BCC7179 preparation containing complementary beta-glucosidase activity. Saccharification yields of 84.0% and 70.4% for glucose and xylose, respectively, were obtained after hydrolysis at 45 degrees C, pH 5 for 72 h, which were slightly higher than those obtained with a commercial enzyme mixture containing Acremonium cellulase and Optimash BG. A high conversion yield of undetoxified pretreated bagasse (5%, w/v) hydrolysate to ethanol was attained by separate hydrolysis and fermentation processes using Pichia stipitis BCC15191, at pH 5.5, 30 degrees C for 24 h resulting in an ethanol concentration of 8.4 g/l, corresponding to a conversion yield of 0.29 g ethanol/g available fermentable sugars. Comparable ethanol conversion efficiency was obtained by a simultaneous saccharification and fermentation process which led to production of 8.0 g/l ethanol after 72 h fermentation under the same conditions. This study thus demonstrated the potential use of a simple integrated process with minimal environmental impact with the use of promising alternative on-site enzymes and yeast for the production of ethanol from this potent lignocellulosic biomass. 2009. Published by Elsevier B.V.

Combined pretreatment using ozonolysis and ball milling to improve enzymatic saccharification of corn straw.

PubMed

Shi, Feng; Xiang, Heji; Li, Yongfu

2015-03-01

Two clean pretreatments, ozonolysis (OZ) and planetary ball milling (BM) were applied separately and in combination to improve the enzymatic hydrolysis of corn straw. Pretreatment of corn straw by OZ and BM alone improved the enzymatic hydrolysis significantly, primarily through delignification and decrystallization of cellulose, respectively. When combined, OZ-BM and BM-OZ pretreatments made the enzymatic hydrolysis more efficient. The glucose and xylose yield of corn straw treated with OZ for 90 min followed by BM for 8 min (OZ90-BM8) reached to 407.8 and 101.9 mg/g-straw, respectively under cellulase loading of 15 FPU/g-straw, which was fivefold more than that of untreated straw. Under much lower cellulase loading of 1.5 FPU/g-straw, the glucose and xylose yield of treated straw OZ90-BM8 remained at 416.0 and 108.4 mg/g-straw, respectively, while the yield of untreated straw decreased. These findings indicate that the combined OZ-BM can be used as a promising pretreatment for corn straw. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effects of Processing Parameters on the Synthesis of (K0.5Na0.5)NbO3 Nanopowders by Reactive High-Energy Ball Milling Method

PubMed Central

Duc Van, Nguyen

2014-01-01

The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C. PMID:24592146

Effects of processing parameters on the synthesis of (K0.5Na0.5)NbO3 nanopowders by reactive high-energy ball milling method.

PubMed

Nguyen, Duc Van

2014-01-01

The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C.

High-energy ball milling technique for ZnO nanoparticles as antibacterial material

PubMed Central

Salah, Numan; Habib, Sami S; Khan, Zishan H; Memic, Adnan; Azam, Ameer; Alarfaj, Esam; Zahed, Nabeel; Al-Hamedi, Salim

2011-01-01

Nanoparticles of zinc oxide (ZnO) are increasingly recognized for their utility in biological applications. In this study, the high-energy ball milling (HEBM) technique was used to produce nanoparticles of ZnO from its microcrystalline powder. Four samples were ball milled for 2, 10, 20, and 50 hours, respectively. The structural and optical modifications induced in the ‘as synthesized’ nanomaterials were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and photoluminescence emission spectra (PL). SEM and TEM results show a gradual decrease in particle size from around 600 to ∼30 nm, with increased milling time. The initial microstructures had random shapes, while the final shape became quite spherical. XRD analysis showed ZnO in a hexagonal structure, broadening in the diffracted peaks and going from larger to smaller particles along with a relaxation in the lattice constant c. The value of c was found to increase from 5.204 to 5.217 Å with a decrease in particle size (600 to ∼30 nm). PL result showed a new band at around 365 nm, whose intensity is found to increase as the particles size decreases. These remarkable structural and optical modifications induced in ZnO nanoparticles might prove useful for various applications. The increase in c value is an important factor for increasing the antibacterial effects of ZnO, suggesting that the HEBM technique is quite suitable for producing these nanoparticles for this purpose. PMID:21720499

Analysis of NO-suppressing activity of Strawberry Wine supplemented with ball-milled achenes.

PubMed

Lee, Pao-Ju; Tsai, Tsung-Yu; Chen, Shaun

2018-04-01

Inflammation is generally thought to be involved in the development of several chronical diseases, therefore, phytochemicals to modulate immune responses has attracted great interests. The objective of the present study was to evaluate the potential anti-inflammatory effects of wine supplemented using ball-milled achene on modulating NO production and inducible nitric oxide synthase (iNOS) expression. Ball-milled achenes were added in strawberry must prior to fermentation, and the wine samples were then concentrated and extracted with water and/or ethanol prior to analysis. Bioactivities of wine extracts were evaluated using the cell viability assay, cell cycle measurements, NO production and iNOS expression in lipopolysaccharide (LPS)-stimulated RAW264.7 cells. Treatments of achenes supplemented strawberry wine extract up to 100 μg/mL inhibited the proliferation of LPS-stimulated RAW264.7 cell via affecting the progression of cell cycle. Moreover, no detectable cytotoxicity in RAW264.7 cells was observed. The supplemented wine extract suppressed the action of LPS and led to a decreased NO production in stimulated cells. The inhibitory effect of the wine extract on NO production was determined to be a 25-40% decrease in the level of 25-100 μg/mL, in contrast to a 10% decrease for conventional wine samples. Additionally, an alcoholic wine extract (100 μg/mL) led to a 40.31% decrease in iNOS expression in LPS-stimulated cells, which was more effective than the same dose of tocopherol. The results show that strawberry wine supplemented with ball-milled achenes causes a substantial inhibition of NO production, and this biofunction is exerted via the down-regulation of iNOS expression.

The Effect of Powder Ball Milling on the Microstructure and Mechanical Properties of Sintered Fe-Cr-Mo-Mn-(Cu) Steel

NASA Astrophysics Data System (ADS)

Kulecki, P.; Lichańska, E.

2017-12-01

The effect of ball milling powder mixtures of Höganäs pre-alloyed iron Astaloy CrM, low-carbon ferromanganese Elkem, elemental electrolytic Cu and C-UF graphite on the sintered structure and mechanical properties was evaluated. The mixing was conducted using Turbula mixer for 30 minutes and CDI-EM60 frequency inverter for 1 and 2 hours. Milling was performed on 150 g mixtures with (in weight %) CrM + 1% Mn, CrM + 2% Mn, CrM + 1% Mn + 1% Cu and CrM + 2% Mn + 1% Cu, all with 0.6%C. The green compacts were single pressed at 660 MPa according to PN-EN ISO 2740. Sintering was carried out in a laboratory horizontal furnace Carbolite STF 15/450 at 1250°C for 60 minutes in 5%H2 - 95%N2 atmosphere with a heating rate of 75°C/min, followed by sintering hardening at 60°C/min cooling rate. All the steels were characterized by martensitic structures. Mechanical testing revealed that steels based on milled powders have slightly higher mechanical properties compared to those only mixed and sintered. The best combination of mechanical properties, for ball milled CrM + 1% Mn + 1% Cu was UTS 1046 MPa, TRS 1336 MPa and A 1.94%.

Grinding arrangement for ball nose milling cutters

NASA Technical Reports Server (NTRS)

Burch, C. F. (Inventor)

1974-01-01

A grinding arrangement for spiral fluted ball nose end mills and like tools includes a tool holder for positioning the tool relative to a grinding wheel. The tool is mounted in a spindle within the tool holder for rotation about its centerline and the tool holder is pivotably mounted for angular movement about an axis which intersects that centerline. A follower arm of a cam follower secured to the spindle cooperates with a specially shaped cam to provide rotation of the tool during the angular movement of the tool holder during the grinding cycle, by an amount determined by the cam profile. In this way the surface of the cutting edge in contact with the grinding wheel is maintained at the same height on the grinding wheel throughout the angular movement of the tool holder during the grinding cycle.

Effect of combination ultrasonic and ball milling techniques of commercial fillers dispersion on mechanical properties of natural rubber (NR) latex films

NASA Astrophysics Data System (ADS)

Hamran, Noramirah; Rashid, Azura A.

2017-07-01

Commercial fillers such as silica and carbon black generally impart the reinforcing effects in dry rubber compound, but have an adverse effect on Natural rubber (NR) latex compounds. The addition of commercial fillers in NR latex has reduced the mechanical properties of NR latex films due to the destabilization effect in the NR latex compounds which govern by the dispersion quality, particle size and also the pH of the dispersion itself. The ball milling process is the conventional meth od of preparation of dispersions and ultrasonic has successfully used in preparation of nano fillers such as carbon nanotube (CNT). In this study the combination between the conventional methods; ball milling together the ultrasonic method were used to prepare the silica and carbon black dispersions. The different duration of ball milling (24, 48 and 72 hours) was compared with the ultrasonic method (30, 60, 90 and 120 minutes). The combination of ball milling and ultrasonic from the optimum individual technique was used to investigate the reduction of particle size of the fillers. The particle size analyzer, transmission electron microscopy (TEM) and scanning electron microscopy (SEM) test were carried out to investigate the obtained particle size and the tensile and tear test were carried out to investigate the mechanical properties of the NR latex films. The reduction of filler particle size is expected to impart the properties of NR latex films.

Nano-Ni induced surface modification relevant to the hydrogenation performances in La-Mg based alloys

NASA Astrophysics Data System (ADS)

Zhang, Huaiwei; Fu, Li; Xuan, Weidong; Li, Xingguo

2018-05-01

Nano-Ni drived modification in LaMg3/Ni composite is investigated. The new phases of LaMg2 and MgNi2 can be formed on the sample surface during the milling process. There is almost no electric charge transfer process between Ni and La element through XPS analyses. The amorphization structure can be found on the alloy surface with the increasing of reaction duration, and the capacity and cycle stability are also greatly promoted. On the other hand, the milled alloys show the lower charge transfer resistance, better anti-corrosion ability and higher oxidation current density.

Low-power, high-uniform, and forming-free resistive memory based on Mg-deficient amorphous MgO film with rough surface

NASA Astrophysics Data System (ADS)

Guo, Jiajun; Ren, Shuxia; Wu, Liqian; Kang, Xin; Chen, Wei; Zhao, Xu

2018-03-01

Saving energy and reducing operation parameter fluctuations remain crucial for enabling resistive random access memory (RRAM) to emerge as a universal memory. In this work, we report a resistive memory device based on an amorphous MgO (a-MgO) film that not only exhibits ultralow programming voltage (just 0.22 V) and low power consumption (less than 176.7 μW) but also shows excellent operative uniformity (the coefficient of variation is only 1.7% and 2.2% for SET and RESET voltage, respectively). Moreover, it also shows a forming-free characteristic. Further analysis indicates that these distinctive properties can be attributed to the unstable local structures and the rough surface of the Mg-deficient a-MgO film. These findings show the potential of using a-MgO in high-performance nonvolatile memory applications.

Synthesis of graphene nanoflakes by grinding natural graphite together with NaCl in a planetary ball mill

NASA Astrophysics Data System (ADS)

Alinejad, Babak; Mahmoodi, Korosh

Natural graphite is a soft material that conventional milling methods fail to grind into nanoparticles. We found that adding NaCl into graphite during milling allows obtaining graphene nanoflakes of about 50×200nm2 as evidenced by Transmission Electron Microscope (TEM). NaCl particles are substantially brittle and harder than graphite, serving as milling agents by both helping to chop graphite into smaller pieces and preventing graphite particles from agglomeration. After milling, NaCl can be easily washed away by water. Probable mechanism for exfoliation of graphene during the modified ball milling may be explained by NaCl and graphene slipping or sliding against and over each other, exfoliating the graphene particles into thin layers.

Improved oral bioavailability of probucol by dry media-milling.

PubMed

Li, Jia; Yang, Yan; Zhao, Meihui; Xu, Hui; Ma, Junyuan; Wang, Shaoning

2017-09-01

The polymer/probucol co-milled mixtures were prepared to improve drug dissolution rate and oral bioavailability. Probucol, a BCS II drug, was co-milled together with Copovidone (Kollidon VA64, VA64), Soluplus, or MCC using the dry media-milling process with planetary ball-milling equipment. The properties of the milled mixtures including morphology, crystal form, vitro drug dissolution and in vivo oral bioavailability in rats were evaluated. Probucol existed as an amorphous in the matrix of the co-milled mixtures containing VA64, which helped to enhance drug dissolution. The ternary mixture composed of VA64, RH40, and probucol showed increased dissolution rates in both sink and non-sink conditions. It also had a higher oral bioavailability compared to the reference formulation. Dry-media milling of binary or ternary mixtures composed of drug, polymer and surfactant possibly have wide applications to improve dissolution rate and oral bioavailability of water-insoluble drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

Atomic simulation of mechanical behavior of Mg in a super-lattice of nanocrystalline Mg and amorphous Mg-Al alloy

NASA Astrophysics Data System (ADS)

Song, H. Y.; An, M. R.; Li, Y. L.; Deng, Q.

2014-12-01

The mechanical properties of a super-lattice architecture composed of nanocrystalline Mg and Mg-Al amorphous alloy are investigated using molecular dynamics simulation. The results indicate that deformation mechanism of nanocrystalline Mg is obviously affected by the amorphous boundary spacing and temperature. The strength of the material increases with the decrease of amorphous boundary spacing, presenting a Hall-Petch effect at both 10 K and 300 K. A stress platform and following stiffness softening, as well as a linear strengthening in the plastic stage, are observed when the amorphous boundary spacing below 8.792 nm at 10 K. The implying reason may be that the amorphous boundary acts as the dislocations emission and absorption source. However, the second stress peak is not observed for the models at 300 K. Instead, the flow stress in plastic stage is a nearly constant value. The simulation demonstrates the emergence of the new grain, accompanied by the deformation twins and stacking faults associated with the plastic behaviors at 300 K. The general conclusions derived from this work may provide a guideline for the design of high-performance hexagonal close-packed metals.

Characterization of Amorphous and Co-Amorphous Simvastatin Formulations Prepared by Spray Drying.

PubMed

Craye, Goedele; Löbmann, Korbinian; Grohganz, Holger; Rades, Thomas; Laitinen, Riikka

2015-12-03

In this study, spray drying from aqueous solutions, using the surface-active agent sodium lauryl sulfate (SLS) as a solubilizer, was explored as a production method for co-amorphous simvastatin-lysine (SVS-LYS) at 1:1 molar mixtures, which previously have been observed to form a co-amorphous mixture upon ball milling. In addition, a spray-dried formulation of SVS without LYS was prepared. Energy-dispersive X-ray spectroscopy (EDS) revealed that SLS coated the SVS and SVS-LYS particles upon spray drying. X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC) showed that in the spray-dried formulations the remaining crystallinity originated from SLS only. The best dissolution properties and a "spring and parachute" effect were found for SVS spray-dried from a 5% SLS solution without LYS. Despite the presence of at least partially crystalline SLS in the mixtures, all the studied formulations were able to significantly extend the stability of amorphous SVS compared to previous co-amorphous formulations of SVS. The best stability (at least 12 months in dry conditions) was observed when SLS was spray-dried with SVS (and LYS). In conclusion, spray drying of SVS and LYS from aqueous surfactant solutions was able to produce formulations with improved physical stability for amorphous SVS.

Phase transformations in amorphous fullerite C60 under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Borisova, P. A.; Blanter, M. S.; Brazhkin, V. V.; Somenkov, V. A.; Filonenko, V. P.

2015-08-01

First phase transformations of amorphous fullerite C60 at high temperatures (up to 1800 K) and high pressures (up to 8 GPa) have been investigated and compared with the previous studies on the crystalline fullerite. The study was conducted using neutron diffraction and Raman spectroscopy. The amorphous fullerite was obtained by ball-milling. We have shown that under thermobaric treatment no crystallization of amorphous fullerite into С60 molecular modification is observed, and it transforms into amorphous-like or crystalline graphite. A kinetic diagram of phase transformation of amorphous fullerite in temperature-pressure coordinates was constructed for the first time. Unlike in crystalline fullerite, no crystalline polymerized phases were formed under thermobaric treatment on amorphous fullerite. We found that amorphous fullerite turned out to be less resistant to thermobaric treatment, and amorphous-like or crystalline graphite were formed at lower temperatures than in crystalline fullerite.

Tungsten solution kinetics and amorphization of nickel in mechanically alloyed Ni-W alloys

NASA Technical Reports Server (NTRS)

Aning, A. O.; Wang, Z.; Courtney, T. H.

1993-01-01

The kinetics of solution of W, and the subsequent amorphization of Ni, in mechanically alloyed Ni-W alloys has been investigated. As W is a highly abrasive material in the energy intensive devices used for mechanical alloying, we studied the above reactions in different mills. One used hardened steel balls as the grinding media, and the other Al2O3. Abrasion is common to both mills, but Fe wear debris from the hardened steel enters into solution in the Ni rich phases whereas Al2O3 debris is present as small dispersoids. The kinetics of W solution and those of subsequent amorphization do not appear strongly affected by the Fe in solution or the Al2O3 dispersoid. Tungsten dissolves in crystalline Ni in amounts in excess of the equilibrium solubility during alloying. Amorphization of the Ni phase occurs if the W content in this phase exceeds ca. 28 at. pct.

Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Omuro, Keisuke; Miura, Harumatsu

1991-05-01

Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

Hydroamination reactions of alkynes with ortho-substituted anilines in ball mills: synthesis of benzannulated N-heterocycles by a cascade reaction.

PubMed

Weiße, Maik; Zille, Markus; Jacob, Katharina; Schmidt, Robert; Stolle, Achim

2015-04-20

It was demonstrated that ortho-substituted anilines are prone to undergo hydroamination reactions with diethyl acetylenedicarboxylate in a planetary ball mill. A sequential coupling of the intermolecular hydroamination reaction with intramolecular ring closure was utilized for the syntheses of benzooxazines, quinoxalines, and benzothiazines from readily available building blocks, that is, electrophilic alkynes and anilines with OH, NH, or SH groups in the ortho position. For the heterocycle formation, it was shown that several stress conditions were able to initiate the reaction in the solid state. Processing in a ball mill seemed to be advantageous over comminution with mortar and pestle with respect to process control. In the latter case, significant postreaction modification occurred during solid-state analysis. Cryogenic milling proved to have an adverse effect on the molecular transformation of the reagents. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Si amorphization by focused ion beam milling: Point defect model with dynamic BCA simulation and experimental validation.

PubMed

Huang, J; Loeffler, M; Muehle, U; Moeller, W; Mulders, J J L; Kwakman, L F Tz; Van Dorp, W F; Zschech, E

2018-01-01

A Ga focused ion beam (FIB) is often used in transmission electron microscopy (TEM) analysis sample preparation. In case of a crystalline Si sample, an amorphous near-surface layer is formed by the FIB process. In order to optimize the FIB recipe by minimizing the amorphization, it is important to predict the amorphous layer thickness from simulation. Molecular Dynamics (MD) simulation has been used to describe the amorphization, however, it is limited by computational power for a realistic FIB process simulation. On the other hand, Binary Collision Approximation (BCA) simulation is able and has been used to simulate ion-solid interaction process at a realistic scale. In this study, a Point Defect Density approach is introduced to a dynamic BCA simulation, considering dynamic ion-solid interactions. We used this method to predict the c-Si amorphization caused by FIB milling on Si. To validate the method, dedicated TEM studies are performed. It shows that the amorphous layer thickness predicted by the numerical simulation is consistent with the experimental data. In summary, the thickness of the near-surface Si amorphization layer caused by FIB milling can be well predicted using the Point Defect Density approach within the dynamic BCA model. Copyright © 2017 Elsevier B.V. All rights reserved.

Thermodynamics, kinetics, and catalytic effect of dehydrogenation from MgH2 stepped surfaces and nanocluster: a DFT study

NASA Astrophysics Data System (ADS)

Reich, Jason; Wang, Linlin; Johnson, Duane

2013-03-01

We detail the results of a Density Functional Theory (DFT) based study of hydrogen desorption, including thermodynamics and kinetics with(out) catalytic dopants, on stepped (110) rutile and nanocluster MgH2. We investigate competing configurations (optimal surface and nanoparticle configurations) using simulated annealing with additional converged results at 0 K, necessary for finding the low-energy, doped MgH2 nanostructures. Thermodynamics of hydrogen desorption from unique dopant sites will be shown, as well as activation energies using the Nudged Elastic Band algorithm. To compare to experiment, both stepped structures and nanoclusters are required to understanding and predict the effects of ball milling. We demonstrate how these model systems relate to the intermediary sized structures typically seen in ball milling experiments.

Synthesis of Multimetal-Graphene Composite by Mechanical Milling

NASA Astrophysics Data System (ADS)

Saiphaneendra, Bachu; Srivastava, Avi Krishna; Srivastava, Chandan

2016-10-01

Multimetal-graphene composites were synthesized using the ball milling technique. To prepare the composite, graphite powder was mixed with Fe, Cr, Co, Cu and Mg powders. This mixture was then mechanically milled for 35 h in toluene medium. After milling, the multimetal-graphite mixture was mixed with sodium lauryl sulfate and sonicated for 2 h. Sonication led to the exfoliation of graphene sheets. Formation of graphene was confirmed from x-ray diffraction and Raman spectroscopy. Transmission electron microscopy-based analysis revealed the formation of multimetal deposits over the graphene surface. Compositional analysis of the multimetal deposits revealed fairly uniform distribution of all the five component metal atoms over the graphene sheet. The average composition of the multimetal deposit was determined to be 11.4 ± 4 at.% Mg, 33.8 ± 19 at.% Cr, 21.8 ± 16 at.% Fe, 9.4 ± 5.7 at.% Co and 23.6 ± 12 at.% Cu.

Surface hardening of Al alloys through controlled ball-milling and sintering.

PubMed

Kim, Seek Hyeoun; Kim, Yong Jin; Ahn, Jung-Ho

2012-07-01

One of the drawbacks of aluminum and its alloys is the lack of proper heat-treatment for surface-hardening. In the present work, a new and simple method of hardening the surface of aluminum and its alloys was developed. Low-energy ball-milling using specific process control agents (PCAs) was employed, using subsequent sintering in a controlled atmosphere. The PCAs in the present work were very effective both for milling and the formation of hard nanocrystalline dispersoids during sintering. The residual oxygen in a sintering atmosphere also played an important role in the formation of AIN or Al-O-N dispersoids. Through the proper control of the processing atmosphere and PCAs, the hardness and thickness of the hardened layers could be adjusted. The results of the wear test showed that the present aluminum alloys can be effectively utilized as light-weight components with a good wear resistance. Furthermore, the present method involves a simple forming process of die-compaction and sintering.

Generation of drugs coated iron nanoparticles through high energy ball milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Radhika Devi, A.; Murty, B. S.; Chelvane, J. A.

The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

Temperature and composition dependence of Mg-based amorphous-alloy structure factors

NASA Astrophysics Data System (ADS)

From, M.; Muir, W. B.

1992-01-01

Measurements of the x-ray total structure factors for amorphous Mg70Zn30, Ca70Mg30, and Mg85.5Cu14.5 at 9, 150, and 300 K have been made. The composition dependence of the room-temperature structure factors of MgxZn1-x have also been measured for values of x=0.65, 0.70, and 0.75. These compositional changes can be accounted for by the increase in average atomic size as the fraction of the larger Mg atoms increases with x. Also the Perkus-Yevick hard-sphere model is sufficient to calculate the change in structure factor with composition if an experimental structure factor is available from which the sphere diameters and packing fraction can be extracted. The temperature dependence of the structure factors is consistent with the observed thermal expansion and a Debye phonon model with Meisel and Cote's approximation for the multiphonon contribution to the structure factor.

The effects of ball size distribution on attritor efficiency

NASA Astrophysics Data System (ADS)

Cook, T. M.; Courtney, T. H.

1995-09-01

A study was undertaken to determine how media dynamics are altered when differently sized grinding balls are used in an attritor. Cinematographic techniques identify the extent of segregation/mixing of the differently sized balls within the attritor as a function of impeller rotational velocity and small ball number fraction. This permits determination of rotational velocities needed to most efficiently use the tactic of milling with differently sized media. Cinematographic observations show that the close-packed media array, assumed when balls of the same size are used for milling, is disrupted when differently sized balls are used. Monitoring powder particle numbers as a function of milling time for the situations when the same and differently sized balls are used can be used to assess relative milling efficiencies. Results indicate powder deformation, fracture, and welding are enhanced through employment of differently sized balls. This conclusion is reinforced by observations of microstructural characteristics of powder processed with the different type of media.

Hydrogenated amorphous carbon films on steel balls and Si substrates: Nanostructural evolutions and their trigging tribological behaviors

NASA Astrophysics Data System (ADS)

Wang, Yongfu; Wang, Yan; Zhang, Xingkai; Shi, Jing; Gao, Kaixiong; Zhang, Bin; Zhang, Junyan

2017-10-01

In this study, we prepared hydrogenated amorphous carbon films on steel balls and Si substrates (steel ball- and Si substrate-films) with different deposition time, and discussed their carbon nanostructural evolutions and tribological behaviors. The steel ball-film structure started to be graphite-like structure and then gradually transformed into fullerene-like (FL) structure. The Si substrate-film structure began in FL structure and kept it through the thickness. The difference may be result from the competition between high starting substrate temperature after additional nitriding applied on the steel balls (its supply power is higher than that in the film deposition), and relaxation of compressive stress from energized ion bombardment in film deposition process. The FL structural film friction couples could achieve ultra-low friction in open air. In particular, the Si substrate-film with 3 h, against the steel ball-film with 2 h and 3 h, exhibited super-low friction (∼0.009) and superlong wear life (∼5.5 × 105 cycles). Our result could widen the superlubricity scope from previously high load and velocity, to middle load and velocity.

Structural and Mössbauer characterization of the ball-milled Fex(Al2O3)100-x system

NASA Astrophysics Data System (ADS)

Paesano, A.; Matsuda, C. K.; Cótica, L. F.; de Medeiros, S. N.; da Cunha, J. B. M.; Hallouche, B.; Silva, S. L.

2004-09-01

Metal-oxide composites were synthesized by high-energy ball milling of metallic iron (α-Fe) and alumina (α-Al2O3) powders, varying the starting relative concentration and the milling time. The samples were characterized by scanning electron microscopy, x-ray diffraction, and Mössbauer spectroscopy. The results revealed the formation of a FeAl2O3+W spinel phase (hercynite) and of iron (super)paramagnetic nanoprecipitates, in addition to residual magnetic iron and alumina. We also observed that the relative amounts of nanoprecipitates and hercynite for isochronally milled samples were correlated with the sample nominal concentration x, with the precursor iron being relatively more converted in those phases for low x values. Particularly for x =10 milled sample, the relative amounts of the (super)paramagnetic and spinel phases were observed to increase linearly with the milling time. An x =20/24h milled sample was annealed in H2 atmosphere and revealed the reduction of hercynite, with iron phase separation.

High energy ball milling study of Fe{sub 2}MnSn Heusler alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jain, Vivek Kumar, E-mail: vivek.jain129@gmail.com; Lakshmi, N.; Jain, Vishal

The structural and magnetic properties of as-melted and high energy ball milled alloy samples have been studied by X-ray diffraction, DC magnetization and electronic structure calculations by means of density functional theory. The observed properties are compared to that of the bulk sample. There is a very good enhancement of saturation magnetization and coercivity in the nano-sized samples as compared to bulk which is explained in terms of structural disordering and size effect.

Solvent-free cross-dehydrogenative coupling reactions under high speed ball-milling conditions applied to the synthesis of functionalized tetrahydroisoquinolines.

PubMed

Su, Weike; Yu, Jingbo; Li, Zhenhua; Jiang, Zhijiang

2011-11-04

Solvent-free reaction using a high-speed ball milling technique has been first applied to cross-dehydrogenative coupling (CDC) reactions between tetrahydroisoquinolines and three types of pronucleophiles such as nitroalkanes, alkynes, and indoles. All coupling products were obtained in good yields at short reaction times (no more than 40 min). When alkynes and indoles were used as pronucleophile, the reactions can be catalyzed efficiently by recoverable copper balls without any additional metal catalyst.

Enhanced Physical Stability of Amorphous Drug Formulations via Dry Polymer Coating.

PubMed

Capece, Maxx; Davé, Rajesh

2015-06-01

Although amorphous solid drug formulations may be advantageous for enhancing the bioavailability of poorly soluble active pharmaceutical ingredients, they exhibit poor physical stability and undergo recrystallization. To address this limitation, this study investigates stability issues associated with amorphous solids through analysis of the crystallization behavior for acetaminophen (APAP), known as a fast crystallizer, using a modified form of the Avrami equation that kinetically models both surface and bulk crystallization. It is found that surface-enhanced crystallization, occurring faster at the free surface than in the bulk, is the major impediment to the stability of amorphous APAP. It is hypothesized that a novel use of a dry-polymer-coating process referred to as mechanical-dry-polymer-coating may be used to inhibit surface crystallization and enhance stability. The proposed process, which is examined, simultaneously mills and coats amorphous solids with polymer, while avoiding solvents or solutions, which may otherwise cause stability or crystallization issues during coating. It is shown that solid dispersions of APAP (64% loading) with a small particle size (28 μm) could be prepared and coated with the polymer, carnauba wax, in a vibratory ball mill. The resulting amorphous solid was found to have excellent stability as a result of inhibition of surface crystallization. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Si@SiOx/Graphene nanosheet anode materials for lithium-ion batteries synthesized by ball milling process

NASA Astrophysics Data System (ADS)

Tie, Xiaoyong; Han, Qianyan; Liang, Chunyan; Li, Bo; Zai, Jiantao; Qian, Xuefeng

2017-12-01

Si@SiOx/Graphene nanosheet (GNS) nanocomposites as high performance anode materials for lithium-ion batteries are synthesized by mechanically blending the mixture of expanded graphite with Si nanoparticles, and characterized by X-ray diffraction, Raman spectrum, field emission scanning electron microscopy and transmission electron microscopy. During the ball milling process, the size of Si nanoparticles will decrease, and the layer of expanded graphite can be peeled off to thin multilayers. Electrochemical performances reveal that the obtained Si@SiOx/GNS nanocomposites exhibit improved cycling stability, high reversible lithium storage capacity and superior rate capability, e.g. the discharge capacity is kept as high as 1055 mAh g-1 within 50 cycles at a current density of 200 mA g-1, retaining 63.6% of the initial value. The high performance of the obtained nanocomposites can be ascribed to GNS prepared through heat-treat and ball-milling methods, the decrease in the size of Si nanoparticles and SiOx layer on Si surface, which enhance the interactions between Si and GNS.

Highly active and stable Ni-Fe bimetal prepared by ball milling for catalytic hydrodechlorination of 4-chlorophenol.

PubMed

Xu, Fuyuan; Deng, Shubo; Xu, Jie; Zhang, Wang; Wu, Min; Wang, Bin; Huang, Jun; Yu, Gang

2012-04-17

A novel Ni-Fe bimetal with high dechlorination activity for 4-chlorophenol (4-CP) was prepared by ball milling (BM) in this study. Increasing Ni content and milling time greatly enhanced the dechlorination activity, which was mainly attributed to the homogeneous distribution of Ni nanoparticles (50-100 nm) in bulk Fe visualized by scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) with image mapping. In comparison with the Ni-Fe bimetal prepared by a chemical solution deposition (CSD) process, the ball milled Ni-Fe bimetal possessed high dechlorination activity and stability before being used up. Dechlorination kinetics indicated that the dechlorination rates of 4-CP increased with increasing Ni-Fe dose but decreased with increasing solution pH. Solution pH had a significant effect on the dechlorination of 4-CP and the passivation of the Ni-Fe bimetal. The enhanced pH during the dechlorination process significantly accelerated the formation of passivating film on the bimetallic surface. The Ni-Fe bimetal at the dose of 60 g/L was reused 10 times without losing dechlorination activity for 4-CP at initial pH less than 6.0, but the gradual passivation was observed at initial pH above 7.0.

Chemical reactions of metal powders with organic and inorganic liquids during ball milling

NASA Technical Reports Server (NTRS)

Arias, A.

1975-01-01

Chromium and/or nickel powders were milled in metal chlorides and in organic liquids representative of various functional groups. The powders always reacted with the liquid and became contaminated with elements from them. The milled powders had specific surface areas ranging from 0.14 to 37 sq m/g, and the total contamination with elements from the milling liquid ranged from 0.01 to 56 weight percent. Compounds resulting from substitution, addition, or elimination reactions formed in or from the milling liquid.

13. TROJAN MILL, INTERIOR SHOWING PRIMARY MILL No. 1 (ALLIS ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

13. TROJAN MILL, INTERIOR SHOWING PRIMARY MILL No. 1 (ALLIS CHALMERS BALL MILL) FROM EAST, c. 1919. ELECTRIC MOTOR AND DRIVE SHAFT CLEARLY VISIBLE. CREDIT WR. - Bald Mountain Gold Mill, Nevada Gulch at head of False Bottom Creek, Lead, Lawrence County, SD

Preparation, characterization and optoelectronic properties of nanodiamonds doped zinc oxide nanomaterials by a ball milling technique

NASA Astrophysics Data System (ADS)

Ullah, Hameed; Sohail, Muhammad; Malik, Uzma; Ali, Naveed; Bangash, Masroor Ahmad; Nawaz, Mohsan

2016-07-01

Zinc oxide (ZnO) is one of the very important metal oxides (MOs) for applications in optoelectronic devices which work in the blue and UV regions. However, to meet the challenges of obtaining ZnO nanomaterials suitable for practical applications, various modifications in physico-chemical properties are highly desirable. One of the ways adopted for altering the properties is to synthesize composite(s) of ZnO with various reinforcements. Here we report on the tuning of optoelectronic properties of ZnO upon doping by nanodiamonds (NDs) using the ball milling technique. A varying weight percent (wt.%) of NDs were ball milled for 2 h with ZnO nanoparticles prepared by a simple precipitation method. The effects of different parameters, the calcination temperature of ZnO, wt.% of NDs and mechanical milling upon the optoelectronic properties of the resulting ZnO-NDs nanocomposites have been investigated. The ZnO-NDs nanocomposites were characterized by IR spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDX). The UV-vis spectroscopy revealed the alteration in the bandgap energy (Eg ) of ZnO as a function of the calcination temperature of ZnO, changing the concentration of NDs, and mechanical milling of the resulting nanocomposites. The photoluminescence (PL) spectroscopy showed a decrease in the deep level emission (DLE) peaks and an increase in near-band-edge transition peaks as a result of the increasing concentration of NDs. The decrease in DLE and increase in band to band transition peaks were due to the strong interaction between the NDs and the Zn+; consequently, the Zn+ concentration decreased on the interstitial sites.

Niobium Carbide-Reinforced Al Matrix Composites Produced by High-Energy Ball Milling

NASA Astrophysics Data System (ADS)

Travessa, Dilermando Nagle; Silva, Marina Judice; Cardoso, Kátia Regina

2017-06-01

Aluminum and its alloys are key materials for the transportation industry as they contribute to the development of lightweight structures. The dispersion of hard ceramic particles in the Al soft matrix can lead to a substantial strengthening effect, resulting in composite materials exhibiting interesting mechanical properties and inspiring their technological use in sectors like the automotive and aerospace industries. Powder metallurgy techniques are attractive to design metal matrix composites, achieving a homogeneous distribution of the reinforcement into the metal matrix. In this work, pure aluminum has been reinforced with particles of niobium carbide (NbC), an extremely hard and stable refractory ceramic. Its use as a reinforcing phase in metal matrix composites has not been deeply explored. Composite powders produced after different milling times, with 10 and 20 vol pct of NbC were produced by high-energy ball milling and characterized by scanning electron microscopy and by X-ray diffraction to establish a relationship between the milling time and size, morphology, and distribution of the particles in the composite powder. Subsequently, an Al/10 pct NbC composite powder was hot extruded into cylindrical bars. The strength of the obtained composite bars is comparable to the commercial high-strength, aeronautical-grade aluminum alloys.

Characterisation of an Al-BN nanocomposite prepared by ball milling and hot extrusion

NASA Astrophysics Data System (ADS)

Arlic, U.; Drozd, Z.; Trojanová, Z.; Molnárová, O.; Kasakewitsch, A.

2017-07-01

Aluminium-matrix-nanocomposites were manufactured by ball milling of microscale aluminium powder with BN nanoparticles in air, followed by subsequent consolidation by hot extrusion. The microstructure of the samples was studied using scanning electron microscopy. Vickers microhardness measurements were used to probe the mechanical properties of the samples. The amplitude dependent damping of the nanocomposites was measured at room temperature after thermal treatment of samples, and the linear thermal expansion was measured over a wide temperature range from room temperature up to 670K in the as-extruded state. The experimental results give a comprehensive picture of the behaviour of this nanocomposite system over the range of thermomechanical treatment conditions examined in this study. Based on these experimental data some possible influences of BN nanoparticles on the anelastic, plastic and thermal properties of microcrystalline aluminium are discussed.

Microstructure characterization and phase transformation kinetic study of ball-milled m-ZrO 2-30 mol% a-TiO 2 mixture by Rietveld method

NASA Astrophysics Data System (ADS)

Pradhan, S. K.; Dutta, H.

2005-05-01

High-energy ball milling of monoclinic ZrO 2-30 mol% anatase TiO 2 mixture at different durations results in the formation of m-ZrO 2-a-TiO 2 solid solution from which the nucleation of nanocrystalline cubic (c) ZrO 2 polymorphic phase sets in. Post-annealing of 12 h ball-milled sample at different elevated temperatures for 1 h results in almost complete formation of c-ZrO 2 phase. Microstructure of the unmilled, all the ball milled and annealed samples has been characterized by Rietveld's X-ray powder structure refinement method. Particle size, rms lattice strain, change in lattice parameters and phase content of individual phases have been estimated from Rietveld analysis, and are utilized to interpret the results. In course of milling, (1 1 1) of cubic lattice became parallel to ( 1bar 1 1) plane of monoclinic lattice due to the orientation effect and cubic phase may have been formed on the (0 0 1) of the m-ZrO 2-a-TiO 2 solid solution lattice. A comparative study of microstructure and phase transformation kinetics of ZrO 2-10, 20 and 30 mol% a-TiO 2 ball-milled and post-annealed samples reveals that rate of phase transformation m→c-ZrO 2 increases with increasing a-TiO 2 concentration and ∼30 mol% of nanocrystalline c-ZrO 2 phase can be obtained within 4 h of milling time in the presence of 30 mol% of a-TiO 2. The post-annealing treatment at 773, 873 and 973 K for 1 h duration each reveals that rate of c-ZrO 2 formation with increasing temperature is retarded with increasing a-TiO 2 concentration but the amount of c-ZrO 2 becomes almost equal (∼95 mol%) at 973 K. It suggests that almost fully stabilized nanocrystalline c-ZrO 2 can be formed by adding a tetravalent solute to m-ZrO 2.

Influence of Iron Oxide Particles on the Strength of Ball-Milled Iron

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lesuer, D R; Syn, C K; Sherby, O D

2005-12-07

Detailed microstructural and mechanical property studies of ball-milled iron, in the powder and consolidated states, are reviewed and assessed. The analyses cover three and one-half orders of magnitude of grain size (from 6 nm to 20 mm) and focus on the influence of oxide particles on the strength. The study includes the early work of Koch and Yang, Kimura and Takaki and continues with the more recent work of Umemoto et al and Belyakov, Sakai et al. It is shown that the major contributors to strength are the nanooxide particles. These particles are created by adiabatic shear banding during ball-millingmore » leading to a bimodal distribution of particles. The predicted strength from particles, {sigma}{sub p}, is given by {sigma}{sub p} = B {center_dot} (D*{sub S}){sup -1/2} where D*{sub S} is the surface-to-surface interparticle spacing, and B = 395 MPa {center_dot} {micro}m{sup -1/2}. A model is proposed that accounts for the influence of the bimodal particle size distribution on strength.« less

Grinding Wear Behaviour of Stepped Austempered Ductile Iron as Media Material During Comminution of Iron Ore in Ball Mills

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raghavendra, H.; Bhat, K. L.; Udupa, K. Rajendra

2011-01-17

An attempt has been made to evaluate the suitability of austempered ductile iron (ADI) as media material for grinding iron ore in a ball mill. Spheroidal graphite (S.G) iron balls are austenitised at 900 deg. C for 60 minutes and given stepped austempering treatment at 280 deg. C for 30 minutes and 60 minutes followed by 380 deg. C for 60 minutes in each case. These materials are characterised by measuring hardness, analysing X-ray diffraction (X-RD), studying microstructure using optical and scanning electron microscope (SEM). Grinding wear behaviour of these materials was assessed for wear loss in wet condition atmore » different pH value of the mineral slurry and found that the wear rate of grinding media material decreases with increase in pH of the slurry. The wear resistance of ADI balls were compared with forged En31 steel balls and found that the stepped austempered ductile iron is superior to forged En31 steel balls.« less

Kinetic study of ferronickel slag grinding at variation of ball filling and ratio of feed to grinding balls

NASA Astrophysics Data System (ADS)

Sanwani, Edy; Ikhwanto, Muhammad

2017-01-01

The objective of this paper is to investigate the effect of ball filling and ratio of feed to grinding balls on the kinetic of grinding of ferronickel slag in a laboratory scale ball mill. The experiments were started by crushing the ferronickel slag samples using a roll crusher to produce -3 mesh (-6.7 mm) product. This product, after sampling and sample dividing processes, was then used as feed for grinding process. The grinding was performed with variations of ball filling and ratio of feed to grinding balls for 150 minutes. At every certain time interval, particle size analysis was carried out on the grinding product. The results of the experiments were also used to develop linear regression model of the effect of grinding variables on the P80 of the product. Based on this study, it was shown that P80 values of the grinding products declined sharply until 70 minutes of grinding time due to the dominant mechanism of impact breakage and then decreased slowly after 70 minutes until 150 minutes of grinding time due to dominant mechanism of attrition breakage. Kinetics study of the grinding process on variations of grinding ball filling showed that the optimum rate of formation of fine particles for 20%, 30%, 40% and 50% mill volume was achieved at a particle size of 400 µm in which the best initial rate of formation occurred at 50% volume of mill. At the variations of ratio of feed to grinding balls it was shown that the optimum rate of grinding for the ratio of 1:10, 1: 8 and 1: 6 was achieved at a particle size of 400 µm and for the ratio of 1: 4 was at 841 µm in which the best initial rate of formation occurred at a 1:10 ratio. In this study, it was also produced two regression models that can predict the P80 value of the grinding product as a function of the variables of grinding time, ball filling and the ratio of the feed to grinding balls.

Dehydriding properties of Ti or/and Zr-doped sodium aluminum hydride prepared by ball-milling

NASA Astrophysics Data System (ADS)

Xiao, Xue-Zhang; Chen, Li-Xin; Wang, Xin-Hua; Li, Shou-Quan; Hang, Zhou-Ming; Chen, Chang-Pin; Wang, Qi-Dong

2007-12-01

The NaAlH4 complex is attracting great attention for its potential applications in hydrogen-powered fuel-cell vehicles due to its high hydrogen storage capacity and suitable thermodynamic properties. However, its practicable hydrogen storage capacity presently obtained is less than the theoretical capacity (5.6 wt.%). To improve the hydrogen capacity, we chose metallic Ti or/and Zr powder as catalyst dopants, and prepared the sodium aluminum hydride by hydrogenation of ball-milled NaH/Al mixture containing 10 mol% dopants with different proportions of Ti and Zr, and then investigated the effects on their hydrogen storage (dehydriding) properties. The results showed that different catalyst dopants affected the dehydriding properties greatly. The catalysis of metal Ti as a catalyst dopant alone on dehydriding kinetics for the entire dehydrogenation process of ball-milled (NaH/Al) composite was higher than that of adopting Zr alone. The synergistic catalytic effect of Ti and Zr together as co-dopants on the dehydrogenation process of (NaH/Al) composite was higher than that using only Ti or Zr as dopant individually. The composite doped with proper proportion of Ti and Zr together (8 mol% Ti+ 2 mol% Zr) as co-dopants exhibited the highest dehydriding kinetic property and desorption capacity.

Research kinetic of motion of milling bodies in ball mill, outfit heat-exchange unit and calculation of its energy performance

NASA Astrophysics Data System (ADS)

Romanovich, A. A.; Romanovich, M. A.; Apukhtina, I. V.

2018-03-01

The article considers topical issues of energy saving in cement production with the use of a technological grinding complex, which includes a press roller grinder and a ball mill. Rational conditions of grinding are proposed for pre-shredded material through the installation of blade energy exchange devices (BEED) in the mill drum. The loading level in the first chamber varies periodically depending on the drum rotation angle, equipped with BEED. In the zone of BEED’s active action, there is a “scooping” of a part of grinding bodies together with crushed material, raising them to a height and giving them a longitudinally transverse movement, which is different from movement created in the mill without BEED. At the same time, additional work that consumes engine power is being done. A technique is proposed for calculating the additional engine power consumption of a mill, equipped with a BEED. This power is spent on creating a longitudinal-transverse motion of grinding bodies and its first and second chambers in areas of active influence of the BEED. Comparative analysis of results obtained experimentally and calculations of proposed equations show a high convergence of results. These analytical dependencies may be interest to Russian and foreign organizations that carry out their activities in the field of design and manufacture of cement equipment, as well as to cement producers.

Influence of ball milling and annealing conditions on the properties of L10 FePt nanoparticles fabricated by a new green chemical synthesis method

NASA Astrophysics Data System (ADS)

Hu, X. C.; Capobianchi, A.; Gallagher, R.; Hadjipanayis, G. C.

2014-05-01

In this work, a new green chemical strategy for the synthesis of L10 FePt alloy nanoparticles is reported. The precursor is a polycrystalline molecular complex (Fe(H2O)6PtCl6), in which Fe and Pt atoms are arranged on alternating planes and milled with NaCl to form nanocrystals. Then the mixture was annealed under reducing atmosphere (5% H2 and 95% Ar) at temperatures varying from 350 °C to 500 °C for 2 h with a heating rate of 5 °C/min. After the reduction, the mixture was washed with water to remove the NaCl and L10 FePt nanoparticles were obtained. The X-Ray Diffraction pattern showed the presence of the characteristic peaks of the fct phase of FePt nanoparticles. Influence of precursor/NaCl ratio and ball milling time on particle size was investigated. Transmission electron microscopy images revealed that smaller precursor/NaCl ratio (10 mg/20 g) and longer milling time (15 h) lead to smaller particle size and narrower size distribution. Milling time does not influence the coercivity much but the decrease of the amount of precursor leads to a decrease of coercivity from 10.8 kOe to 4.8 kOe.

Amorphous InGaMgO Ultraviolet Photo-TFT with Ultrahigh Photosensitivity and Extremely Large Responsivity

PubMed Central

Zhang, Yiyu; Qian, Ling-Xuan; Wu, Zehan; Liu, Xingzhao

2017-01-01

Recently, amorphous InGaZnO ultraviolet photo thin-film transistors have exhibited great potential for application in future display technologies. Nevertheless, the transmittance of amorphous InGaZnO (~80%) is still not high enough, resulting in the relatively large sacrifice of aperture ratio for each sensor pixel. In this work, the ultraviolet photo thin-film transistor based on amorphous InGaMgO, which processes a larger bandgap and higher transmission compared to amorphous InGaZnO, was proposed and investigated. Furthermore, the effects of post-deposition annealing in oxygen on both the material and ultraviolet detection characteristics of amorphous InGaMgO were also comprehensively studied. It was found that oxygen post-deposition annealing can effectively reduce oxygen vacancies, leading to an optimized device performance, including lower dark current, higher sensitivity, and larger responsivity. We attributed it to the combined effect of the reduction in donor states and recombination centers, both of which are related to oxygen vacancies. As a result, the 240-min annealed device exhibited the lowest dark current of 1.7 × 10−10 A, the highest photosensitivity of 3.9 × 106, and the largest responsivity of 1.5 × 104 A/W. Therefore, our findings have revealed that amorphous InGaMgO photo thin-film transistors are a very promising alternative for UV detection, especially for application in touch-free interactive displays. PMID:28772529

Amorphous InGaMgO Ultraviolet Photo-TFT with Ultrahigh Photosensitivity and Extremely Large Responsivity.

PubMed

Zhang, Yiyu; Qian, Ling-Xuan; Wu, Zehan; Liu, Xingzhao

2017-02-13

Recently, amorphous InGaZnO ultraviolet photo thin-film transistors have exhibited great potential for application in future display technologies. Nevertheless, the transmittance of amorphous InGaZnO (~80%) is still not high enough, resulting in the relatively large sacrifice of aperture ratio for each sensor pixel. In this work, the ultraviolet photo thin-film transistor based on amorphous InGaMgO, which processes a larger bandgap and higher transmission compared to amorphous InGaZnO, was proposed and investigated. Furthermore, the effects of post-deposition annealing in oxygen on both the material and ultraviolet detection characteristics of amorphous InGaMgO were also comprehensively studied. It was found that oxygen post-deposition annealing can effectively reduce oxygen vacancies, leading to an optimized device performance, including lower dark current, higher sensitivity, and larger responsivity. We attributed it to the combined effect of the reduction in donor states and recombination centers, both of which are related to oxygen vacancies. As a result, the 240-min annealed device exhibited the lowest dark current of 1.7 × 10 -10 A, the highest photosensitivity of 3.9 × 10⁶, and the largest responsivity of 1.5 × 10⁴ A/W. Therefore, our findings have revealed that amorphous InGaMgO photo thin-film transistors are a very promising alternative for UV detection, especially for application in touch-free interactive displays.

Quenching ilmenite with a high-temperature and high-pressure phase using super-high-energy ball milling.

PubMed

Hashishin, Takeshi; Tan, Zhenquan; Yamamoto, Kazuhiro; Qiu, Nan; Kim, Jungeum; Numako, Chiya; Naka, Takashi; Valmalette, Jean Christophe; Ohara, Satoshi

2014-04-25

The mass production of highly dense oxides with high-temperature and high-pressure phases allows us to discover functional properties that have never been developed. To date, the quenching of highly dense materials at the gramme-level at ambient atmosphere has never been achieved. Here, we provide evidence of the formation of orthorhombic Fe2TiO4 from trigonal FeTiO3 as a result of the high-temperature (>1250 K) and high-pressure (>23 GPa) condition induced by the high collision energy of 150 gravity generated between steel balls. Ilmenite was steeply quenched by the surrounding atmosphere, when iron-rich ilmenite (Fe2TiO4) with a high-temperature and high-pressure phase was formed by planetary collisions and was released from the collision points between the balls. Our finding allows us to infer that such intense planetary collisions induced by high-energy ball milling contribute to the mass production of a high-temperature and high-pressure phase.

Quenching ilmenite with a high-temperature and high-pressure phase using super-high-energy ball milling

PubMed Central

Hashishin, Takeshi; Tan, Zhenquan; Yamamoto, Kazuhiro; Qiu, Nan; Kim, Jungeum; Numako, Chiya; Naka, Takashi; Valmalette, Jean Christophe; Ohara, Satoshi

2014-01-01

The mass production of highly dense oxides with high-temperature and high-pressure phases allows us to discover functional properties that have never been developed. To date, the quenching of highly dense materials at the gramme-level at ambient atmosphere has never been achieved. Here, we provide evidence of the formation of orthorhombic Fe2TiO4 from trigonal FeTiO3 as a result of the high-temperature (>1250 K) and high-pressure (>23 GPa) condition induced by the high collision energy of 150 gravity generated between steel balls. Ilmenite was steeply quenched by the surrounding atmosphere, when iron-rich ilmenite (Fe2TiO4) with a high-temperature and high-pressure phase was formed by planetary collisions and was released from the collision points between the balls. Our finding allows us to infer that such intense planetary collisions induced by high-energy ball milling contribute to the mass production of a high-temperature and high-pressure phase. PMID:24763088

Fe-FeS2 adsorbent prepared with iron powder and pyrite by facile ball milling and its application for arsenic removal.

PubMed

Min, Xiaobo; Li, Yangwenjun; Ke, Yong; Shi, Meiqing; Chai, Liyuan; Xue, Ke

2017-07-01

Arsenic is one of the major pollutants and a worldwide concern because of its toxicity and chronic effects on human health. An adsorbent of Fe-FeS 2 mixture for effective arsenic removal was successfully prepared by mechanical ball milling. The products before and after arsenic adsorption were characterized with scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The adsorbent shows high arsenic removal efficiency when molar ratio of iron to pyrite is 5:5. The experimental data of As(III) adsorption are fitted well with the Langmuir isotherm model with a maximal adsorption capacity of 101.123 mg/g. And As(V) data were described perfectly by the Freundlich model with a maximal adsorption capacity of 58.341 L/mg. As(III) is partial oxidized to As(V) during the adsorption process. High arsenic uptake capability and cost-effectiveness of waste make it potentially attractive for arsenic removal.

Hydrogen kinetics studies of MgH2-FeTi composites

NASA Astrophysics Data System (ADS)

Meena, Priyanka; Jangir, Mukesh; Singh, Ramvir; Sharma, V. K.; Jain, I. P.

2018-05-01

MgH2 + x wt% FeTi (x=10, 25, 50) nano composites were ball milled to get nano structured material and characterized for structural, morphological and thermal properties. XRD of the milled samples revealed the formation of MgH2, FeTi, Fe2Ti and H0.06FeTi phases. Morphological studies by SEM were undertaken to investigate the effect of hydrogenation of nanostructure alloy. EDX confirmed elemental composition of the as-prepared alloy. TGA studies showed higher desorption temperature for milled MgH2 compared to x wt% FeTi added MgH2. Activation energy for hydrogen desorption was found to be -177.90, -215.69, -162.46 and -87.93 kJ/mol for milled MgH2 and Mg2+x wt% FeTi (10, 25, 50), showing 89.97 kJ/ mol reduction in activation energy for 50 wt% alloy additives resulting in improved hydrogen storage capacity. DSC investigations were carried out to investigate the effect of alloy on hydrogen absorption behavior of MgH2.

Preparation of MgB2 superconducting microbridges by focused ion beam direct milling

NASA Astrophysics Data System (ADS)

Zhang, Xuena; Li, Yanli; Xu, Zhuang; Kong, Xiangdong; Han, Li

2017-01-01

MgB2 superconducting microbridges were prepared by focused ion beam (FIB) direct milling on MgB2 films. The surface topography of the microbridges were observed using SEM and AFM and the superconductivity was measured in this paper. Lots of cracks and holes were found near the milled area. And the superconducting transition temperature was decreased a lot and the bridges prepared were not superconducting due to ion damage after milled with large dose. Through these works, we explored the effect regular of FIB milling and experimental parameters on the performance of microbridges.

Development of a Hydrogen Uptake-Release Mg-Based Alloy by Adding a Polymer CMC (Carboxymethylcellulose, Sodium Salt) via Reaction-Accompanying Milling

NASA Astrophysics Data System (ADS)

Kwak, Young Jun; Choi, Eunho; Song, Myoung Youp

2018-03-01

The addition of carboxymethylcellulose, sodium salt (CMC) might improve the hydrogen uptake and release properties of Mg since it has a relatively low melting point and the melting of CMC during milling in hydrogen (reaction-accompanying milling) may make the milled samples be in good states to absorb and release hydrogen rapidly and to have a large hydrogen-storage capacity. Samples with compositions of 95 w/o Mg + 5 w/o CMC (named Mg-5CMC) and 90 w/o Mg + 10 w/o CMC (named Mg-10CMC) were prepared by adding CMC via reaction-accompanying milling. Activation of Mg-10CMC was completed after about 3 hydrogen uptake-release cycles. Mg-10CMC had a higher initial hydrogen uptake rate and a larger amount of hydrogen absorbed in 60 min, U (60 min), than Mg-5CMC before and after activation. At the cycle number of three (CN = 3), Mg-10CMC had a very high initial hydrogen uptake rate (1.56 w/o H/min) and a large U (60 min) (5.57 w/o H) at 593 K in hydrogen of 12 bar, showing that the activated Mg-10CMC has an effective hydrogen-storage capacity of about 5.6 w/o at 593 K in hydrogen of 12 bar at CN = 3. At CN = 2, Mg-10CMC released 1.00 w/o H in 2.5 min, 4.67 w/o H in 10 min, and 4.76 w/o H in 60 min at 648 K in hydrogen of 1.0 bar. The milling in hydrogen of Mg with CMC is believed to generate imperfections and cracks and reduce the particle size. The addition of 10 w/o CMC was more effective on the initial hydrogen uptake rate and U (60 min) compared with the 10 w/o additions of NbF5, TaF5, Fe2O3, and MnO, and the 10 w/o simultaneous addition of Ni, Fe, and Ti. To the best of our knowledge, this study is the first in which a polymer CMC is added to Mg by reaction-accompanying milling to improve the hydrogen storage properties of Mg.

Magnetic Properties of Amorphous Fe-Si-B Powder Cores Mixed with Pure Iron Powder

NASA Astrophysics Data System (ADS)

Kim, Hyeon-Jun; Nam, Seul Ki; Kim, Kyu-Sung; Yoon, Sung Chun; Sohn, Keun-Yong; Kim, Mi-Rae; Sul Song, Yong; Park, Won-Wook

2012-10-01

Amorphous Fe-Si-B alloy was prepared by melt-spinning, and then the ribbons were pulverized and ball-milled to make the amorphous powder of ˜25 µm in size. Subsequently those were mixed with pure iron powders with an average particle size of 3 µm, and 1.5 wt % water glass diluted by distilled water at the ratio of 1:2. The powder mixtures were cold compacted at 650 MPa in toroid die, and heat treated at 430-440 °C under a nitrogen atmosphere for 1 h and 30 min, respectively. The soft magnetic properties of powder core were investigated using a B-H analyzer and a flux meter at the frequency range of ˜100 kHz. The microstructure was observed using scanning electron microscope (SEM), and the density of the core was measured using the principle of Archimedes. Based on the experimental results, the amorphous powder mixed with pure iron powder showed the improved powder compactability, which resulted in the increased permeability and the reduced core loss.

Microwave Absorption Properties of Iron Nanoparticles Prepared by Ball-Milling

NASA Astrophysics Data System (ADS)

Chu, Xuan T. A.; Ta, Bach N.; Ngo, Le T. H.; Do, Manh H.; Nguyen, Phuc X.; Nam, Dao N. H.

2016-05-01

A nanopowder of iron was prepared using a high-energy ball milling method, which is capable of producing nanoparticles at a reasonably larger scale compared to conventional chemical methods. Analyses using x-ray diffraction and magnetic measurements indicate that the iron nanoparticles are a single phase of a body-centered cubic structure and have quite stable magnetic characteristics in the air. The iron nanoparticles were then mixed with paraffin and pressed into flat square plates for free-space microwave transmission and reflection measurements in the 4-8 GHz range. Without an Al backing plate, the Fe nanoparticles seem to only weakly absorb microwave radiation. The reflected signal S 11 drops to zero and a very large negative value of reflection loss ( RL) are observed for Al-backed samples, suggesting the existence of a phase matching resonance near frequency f ˜ 6 GHz.

Preparation of TiO2-Decorated Boron Particles by Wet Ball Milling and their Photoelectrochemical Hydrogen and Oxygen Evolution Reactions

PubMed Central

Jung, Hye Jin; Nam, Kyusuk; Sung, Hong-Gye; Hyun, Hyung Soo; Sohn, Youngku; Shin, Weon Gyu

2016-01-01

TiO2-coated boron particles were prepared by a wet ball milling method, with the particle size distribution and average particle size being easily controlled by varying the milling operation time. Based on the results from X-ray photoelectron spectroscopy, transmission electron microscopy, energy dispersive X-ray analysis, and Fourier transform infrared spectroscopy, it was confirmed that the initial oxide layer on the boron particles surface was removed by the wet milling process, and that a new B–O–Ti bond was formed on the boron surface. The uniform TiO2 layer on the 150 nm boron particles was estimated to be 10 nm thick. Based on linear sweep voltammetry, cyclic voltammetry, current-time amperometry, and electrochemical impedance analyses, the potential for the application of TiO2-coated boron particles as a photoelectrochemical catalyst was demonstrated. A current of 250 μA was obtained at a potential of 0.5 V for hydrogen evolution, with an onset potential near to 0.0 V. Finally, a current of 220 μA was obtained at a potential of 1.0 V for oxygen evolution. PMID:28774132

Determination of rational parameters for process of grinding materials pre-crushed by pressure in ball mill

NASA Astrophysics Data System (ADS)

Romanovich, A. A.; Romanovich, L. G.; Chekhovskoy, E. I.

2018-03-01

The article presents the results of experimental studies on the grinding process of a clinker preliminarily ground in press roller mills in a ball mill equipped with energy exchange devices. The authors studied the influence of the coefficients of loading for grinding bodies of the first and second mill chambers, their lengths, angles of inclination, and the mutual location of energy exchange devices (the ellipse segment and the double-acting blade) on the output parameters of the grinding process (productivity, drive power consumption and specific energy consumption). It is clarified that the best results of the disaggregation and grinding process, judging by the minimum specific energy consumption in the grinding of clinker with an anisotropic texture after force deformation between the rolls of a press roller shredder, are achieved at a certain angle of ellipse segment inclination; the length of the first chamber and the coefficients of loading the chambers with grinding bodies.

Milling induced amorphisation and recrystallization of α-lactose monohydrate.

PubMed

Badal Tejedor, Maria; Pazesh, Samaneh; Nordgren, Niklas; Schuleit, Michael; Rutland, Mark W; Alderborn, Göran; Millqvist-Fureby, Anna

2018-02-15

Preprocessing of pharmaceutical powders is a common procedure to condition the materials for a better manufacturing performance. However, such operations may induce undesired material properties modifications when conditioning particle size through milling, for example. Modification of both surface and bulk material structure will change the material properties, thus affecting the processability of the powder. Hence it is essential to control the material transformations that occur during milling. Topographical and mechanical changes in surface properties can be a preliminary indication of further material transformations. Therefore a surface evaluation of the α-lactose monohydrate after short and prolonged milling times has been performed. Unprocessed α-lactose monohydrate and spray dried lactose were evaluated in parallel to the milled samples as reference examples of the crystalline and amorphous lactose structure. Morphological differences between unprocessed α-lactose, 1 h and 20 h milled lactose and spray dried lactose were detected from SEM and AFM images. Additionally, AFM was used to simultaneously characterize particle surface amorphicity by measuring energy dissipation. Extensive surface amorphicity was detected after 1 h of milling while prolonged milling times showed only a moderate particle surface amorphisation. Bulk material characterization performed with DSC indicated a partial amorphicity for the 1 h milled lactose and a fully amorphous thermal profile for the 20 h milled lactose. The temperature profiles however, were shifted somewhat in the comparison to the amorphous reference, particularly after extended milling, suggesting a different amorphous state compared to the spray-dried material. Water loss during milling was measured with TGA, showing lower water content for the lactose amorphized through milling compared to spray dried amorphous lactose. The combined results suggest a surface-bulk propagation of the amorphicity during

Methods of amorphization and investigation of the amorphous state.

PubMed

Einfal, Tomaž; Planinšek, Odon; Hrovat, Klemen

2013-09-01

The amorphous form of pharmaceutical materials represents the most energetic solid state of a material. It provides advantages in terms of dissolution rate and bioavailability. This review presents the methods of solid- -state amorphization described in literature (supercooling of liquids, milling, lyophilization, spray drying, dehydration of crystalline hydrates), with the emphasis on milling. Furthermore, we describe how amorphous state of pharmaceuticals differ depending on the method of preparation and how these differences can be screened by a variety of spectroscopic (X-ray powder diffraction, solid state nuclear magnetic resonance, atomic pairwise distribution, infrared spectroscopy, terahertz spectroscopy) and calorimetry methods.

Influence of B4C-doping and high-energy ball milling on phase formation and critical current density of (Bi,Pb)-2223 HTS

NASA Astrophysics Data System (ADS)

Margiani, N. G.; Mumladze, G. A.; Adamia, Z. A.; Kuzanyan, A. S.; Zhghamadze, V. V.

2018-05-01

In this paper, the combined effects of B4C-doping and planetary ball milling on the phase evolution, microstructure and transport properties of Bi1.7Pb0.3Sr2Ca2Cu3Oy(B4C)x HTS with x = 0 ÷ 0.125 were studied through X-ray diffraction (XRD), scanning electron microscopy (SEM), resistivity and critical current density measurements. Obtained results have shown that B4C additive leads to the strong acceleration of high-Tc phase formation and substantial enhancement in Jc. High-energy ball milling seems to produce a more homogeneous distribution of refined doped particles in the (Bi,Pb)-2223 HTS which results in an improved intergranular flux pinning and better self-field Jc performance.

Nitrogen-doped graphene catalysts: High energy wet ball milling synthesis and characterizations of functional groups and particle size variation with time and speed

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhuang, Shiqiang; Nunna, Bharath Babu; Boscoboinik, Jorge Anibal

Nitrogen-doped graphene (N-G) catalyst emerges as one of the promising non-platinum group metal (non-PGM) catalysts with the advantages of low cost, high oxygen reduction reaction (ORR) activity, stability, and selectivity to replace expensive PGM catalysts in electrochemical systems. This research investigated nanoscale high energy wet (NHEW) ball milling for the synthesis of N-G catalysts to make conventional problems such as sintering or localized overheating issues negligible. The successful synthesis of N-G catalysts with comparable catalytic performance to 10 wt% Pt/C by using this method has been published. This paper focuses on understanding the effect of grinding speed and grinding timemore » on the particle size and chemical state of N-G catalysts through the physical and chemical characterization. The research result shows that (1) the final particle size, nitrogen doping percentage, and nitrogen bonding composition of synthesized N-G catalysts are predictable and controllable by adjusting the grinding time, the grinding speed, and other relative experimental parameters; (2) the final particle size of N-G catalysts could be estimated from the derived relation between the cracking energy density and the particle size of ground material in the NHEW ball milling process with specified experimental parameters; and (3) the chemical composition of N-G catalysts synthesized by NHEW ball milling is controllable by adjusting the grinding time and grinding speed.« less

Nitrogen-doped graphene catalysts: High energy wet ball milling synthesis and characterizations of functional groups and particle size variation with time and speed

DOE PAGES

Zhuang, Shiqiang; Nunna, Bharath Babu; Boscoboinik, Jorge Anibal; ...

2017-07-26

Nitrogen-doped graphene (N-G) catalyst emerges as one of the promising non-platinum group metal (non-PGM) catalysts with the advantages of low cost, high oxygen reduction reaction (ORR) activity, stability, and selectivity to replace expensive PGM catalysts in electrochemical systems. This research investigated nanoscale high energy wet (NHEW) ball milling for the synthesis of N-G catalysts to make conventional problems such as sintering or localized overheating issues negligible. The successful synthesis of N-G catalysts with comparable catalytic performance to 10 wt% Pt/C by using this method has been published. This paper focuses on understanding the effect of grinding speed and grinding timemore » on the particle size and chemical state of N-G catalysts through the physical and chemical characterization. The research result shows that (1) the final particle size, nitrogen doping percentage, and nitrogen bonding composition of synthesized N-G catalysts are predictable and controllable by adjusting the grinding time, the grinding speed, and other relative experimental parameters; (2) the final particle size of N-G catalysts could be estimated from the derived relation between the cracking energy density and the particle size of ground material in the NHEW ball milling process with specified experimental parameters; and (3) the chemical composition of N-G catalysts synthesized by NHEW ball milling is controllable by adjusting the grinding time and grinding speed.« less

Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching.

PubMed

Swain, Basudev; Mishra, Chinmayee; Kang, Leeseung; Park, Kyung-Soo; Lee, Chan Gi; Hong, Hyun Seon

2015-04-01

Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na2CO3, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na2CO3, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4M HCl, 100°C and pulp density of 20g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching. Copyright © 2015 Elsevier Inc. All rights reserved.

Morphological and XPS study of ball milled Fe1-xAlx (0.3≤x≤0.6) alloys

NASA Astrophysics Data System (ADS)

Rajan, Sandeep; Kumar, Anil; Vyas, Anupam; Brajpuriya, Ranjeet

2018-05-01

The paper presents mechanical and XPS study of ball milled Fe1-xAlx (0.3≤x≤0.6) alloys. The author prepared the solid solution of Fe(Al) with different composition of Al by using mechanical alloying (MA) technique. The MA process induces a progressive dissolution of Al into Fe, resulted in the formation of an extended Fe(Al) solid solution with the bcc structure after 5 hr of milling. The SEM Images shows that the initial shape of particles disappeared completely, and their structure became a mixture of small and large angular-shaped crystallites with different sizes. The TEM micrograph also confirms the reduction in crystallite size and alloy formation. XPS study shows the shift in the binding energy position of both Fe and Al Peaks provide strong evidence of Fe(Al) phase formation after milling.

The reduction of optimal heat treatment temperature and critical current density enhancement of ex situ processed MgB2 tapes using ball milled filling powder

NASA Astrophysics Data System (ADS)

Fujii, Hiroki; Iwanade, Akio; Kawada, Satoshi; Kitaguchi, Hitoshi

2018-01-01

The optimal heat treatment temperature (Topt) at which best performance in the critical current density (Jc) property at 4.2 K is obtained is influenced by the quality or reactivity of the filling powder in ex situ processed MgB2 tapes. Using a controlled fabrication process, the Topt decreases to 705-735 °C, which is lower than previously reported by more than 50 °C. The Topt decrease is effective to suppress both the decomposition of MgB2 and hence the formation of impurities such as MgB4, and the growth of crystallite size which decreases upper critical filed (Hc2). These bring about the Jc improvement and the Jc value at 4.2 K and 10 T reaches 250 A/mm2. The milling process also decreases the critical temperature (Tc) below 30 K. The milled powder is easily contaminated in air and thus, the Jc property of the contaminated tapes degrades severely. The contamination can raise the Topt by more than 50 °C, which is probably due to the increased sintering temperature required against contaminated surface layer around the grains acting as a barrier.

The use of inverse phase gas chromatography to study the change of surface energy of amorphous lactose as a function of relative humidity and the processes of collapse and crystallisation.

PubMed

Newell, H E; Buckton, G; Butler, D A; Thielmann, F; Williams, D R

2001-04-17

The purpose of this study was to assess the effect of relative humidity (RH) on the surface energy of amorphous lactose. Two samples of amorphous lactose were investigated; a spray dried 100% amorphous material and a ball milled sample of crystalline lactose. The milled sample had less than 1% amorphous content by mass, but on investigation at 0% RH, yielded surface energies comparable to those obtained from the 100% amorphous material, indicating that the surface was amorphous. The effect of increasing humidity was to reduce the dispersive surface energy of the two samples from 36.0 +/- 0.14 and 41.6 +/- 1.4 mJ m(-2) at 0% RH for the spray dried and milled samples respectively, to a value comparable to that obtained for the crystalline alpha-lactose monohydrate of 31.3 +/- 0.41 mJ m(-2). The change in surface energy due to water sorption was only reversible up to 20% RH; after exposure to higher RH values subsequent drying did not result in a return to the original surface energy of the amorphous form. This shows that the surface is reorganising as the glass transition temperature (Tg) is reduced, even though the sample has not collapsed or crystallised. It was possible to follow the collapse behaviour in the column with ease, using a number of different methods.

Structural and phase transformations during ball milling of titanium in medium of liquid hydrocarbons

NASA Astrophysics Data System (ADS)

Dorofeev, G. A.; Lubnin, A. N.; Lad'yanov, V. I.; Mukhgalin, V. V.; Puskkarev, B. E.

2014-02-01

It has been shown using X-ray diffraction, scanning electron microscopy, and chemical analysis that, upon ball milling of α-titanium in liquid organic media (toluene and n-heptane), a nanocrystalline fcc phase is formed that is a metastable carbohydride Ti(C,H) deficient in hydrogen and carbon compared to stable carbohydrides. The dimensions of powder particles after milling in toluene and n-heptane differ substantially (are 5-10 and 20-30 μm, respectively. It has been shown that the kinetics of the formation of Ti(C,H) is independent of the milling medium. The atomic ratios H/C in the products of mechanosynthesis agree well with those corresponding to the employed organic media, i.e., H/C = 1.1 for toluene and 2.3 for n-heptane. A solid-liquid mechanism of mechanosynthesis is suggested, which includes repeated processes of particle fracturing with the formation of fresh surfaces, adsorption of liquid hydrocarbons on these surfaces, and subsequent cold welding of the newly formed particles. It is assumed that the formation of the fcc phase in the process of milling is connected with the generation of stacking faults in α-Ti. Upon annealing at 550°C, the fcc phase decomposes with the formation of stable titanium carbide TiC (annealing in a vacuum) or stable titanium carbohydride and a β-Ti(H) solid solution (annealing in argon) with a partial reverse transformation Ti(C,H) → α-Ti in both cases.

Improved hydrogen storage properties of MgH2 catalyzed with TiO2

NASA Astrophysics Data System (ADS)

Jangir, Mukesh; Meena, Priyanka; Jain, I. P.

2018-05-01

In order to improve the hydrogenation properties of the MgH2, various concentration of rutile Titanium Oxide (TiO2) (X wt%= 5, 10, 15 wt %) is added to MgH2 by ball milling and the catalytic effect of TiO2 on hydriding/dehydriding properties of MgH2 has been investigated. Result shows that the TiO2 significantly reduced onset temperature of desorption. Onset temperature as low as 190 °C were observed for the MgH2-15 wt% TiO2 sample which is 60 °C and 160 °C lower than the as-milled and as-received MgH2. Fromm the Kissinger plot the activation energy of 15 wt% TiO2 added sample is calculated to be -75.48 KJ/mol. These results indicate that the hydrogenation properties of MgH2-TiO2 have been improved compared to the as-milled and as-received MgH2. Furthermore, XRD and XPS were performed to characterize the structural evolution upon milling and dehydrogenation.

Highly Al-doped TiO{sub 2} nanoparticles produced by Ball Mill Method: structural and electronic characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Santos, Desireé M. de los, E-mail: desire.delossantos@uca.es; Navas, Javier, E-mail: javier.navas@uca.es; Sánchez-Coronilla, Antonio

2015-10-15

Highlights: • Highly Al-doped TiO{sub 2} nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO{sub 2} nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy.more » The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti{sup 4+} ions by Al{sup 3+} in the TiO{sub 2} lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature.« less

Structural and Mössbauer characterization of the ball milled Fe x(Cr 2O 3) 1- x system

NASA Astrophysics Data System (ADS)

Biondo, Valdecir; de Medeiros, Suzana Nóbrega; Paesano, Andrea, Jr.; Ghivelder, Luis; Hallouche, Bachir; da Cunha, João Batista Marimon

2009-08-01

The Fe x(Cr 2O 3) 1- x system, with 0.10 ≤ X ≤ 0.80, was mechanically processed for 24 h in a high-energy ball-mill. In order to examine the possible formation of iron-chromium oxides and alloys, the milled samples were, later, thermally annealed in inert (argon) and reducing (hydrogen) atmospheres. The as-milled and annealed products were characterized by X-ray diffraction, Mössbauer spectroscopy, transmission electron microscopy and magnetization. The as-milled samples showed the formation of an Fe 1+ YCr 2- YO 4- δ nanostructured and disordered spinel phase, the α 1-Fe(Cr) and α 2-Cr(Fe) solid solutions and the presence of non-exhausted precursors. For the samples annealed in inert atmosphere, the chromite (FeCr 2O 4) formation and the recrystallization of the precursors were verified. The hydrogen treated samples revealed the reduction of the spinel phase, with the phase separation of the chromia phase and retention of the Fe-Cr solid solutions. All the samples, either as-milled or annealed, presented the magnetization versus applied field curves typical for superparamagnetic systems.

Aerodynamic Resistance of a Ball-Tube Mill During Transport of a Polydisperse Coal Gas Suspension

NASA Astrophysics Data System (ADS)

Ivanov, S. D.; Kudryashov, A. N.; Oshchepkov, V. V.

2018-03-01

Analysis of experimental data on aerodynamic resistance of a ball-tube mill is given. It is shown that this resistance has two components brought about by the pressure losses resulting from the injection of dust particles into the main flow after coal grinding and from the transport of homogeneous gas suspension flow. A dimensionless equation has been obtained for the dependence of the pressure loss in flow of a homogeneous dust-air mixture on Reynolds number. Functional dependences of the mean-square velocity of the floating of coal particles and of their average diameter on the polydispersity parameters of coal dust have been found. An empirical dependence of pressure loss due to the injection of a polydisperse coal gas suspension into the main flow on the average velocity of floating of coal particles, their average size, and on the size of the mill has been obtained.

Aerodynamic Resistance of a Ball-Tube Mill During Transport of a Polydisperse Coal Gas Suspension

NASA Astrophysics Data System (ADS)

Ivanov, S. D.; Kudryashov, A. N.; Oshchepkov, V. V.

2018-05-01

Analysis of experimental data on aerodynamic resistance of a ball-tube mill is given. It is shown that this resistance has two components brought about by the pressure losses resulting from the injection of dust particles into the main flow after coal grinding and from the transport of homogeneous gas suspension flow. A dimensionless equation has been obtained for the dependence of the pressure loss in flow of a homogeneous dust-air mixture on Reynolds number. Functional dependences of the mean-square velocity of the floating of coal particles and of their average diameter on the polydispersity parameters of coal dust have been found. An empirical dependence of pressure loss due to the injection of a polydisperse coal gas suspension into the main flow on the average velocity of floating of coal particles, their average size, and on the size of the mill has been obtained.

Processing and Characterization of Fe-Mn-Cu-Sn-C Alloys Prepared by Ball Milling and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Bączek, Elżbieta; Konstanty, Janusz; Romański, Andrzej; Podsiadło, Marcin; Cyboroń, Jolanta

2018-03-01

In this work, Fe-Mn-Cu-Sn-C alloys were prepared by means of powder metallurgy (PM). Powder mixtures were ball-milled for 8, 30 and 120 h and densified to < 1% porosity using spark plasma sintering (SPS) at 900 °C and 35 MPa. After consolidation, all samples of the Fe alloys were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), hardness and flexural strength tests. Resistance to abrasive wear was evaluated in both three-body abrasion and two-body abrasion tests. The SEM observations revealed an evident dependence of grain size and microstructural homogeneity on milling time. The XRD analysis showed a marked increase in austenite content in the as-sintered specimens with milling time. Although the proportion of deformation-induced martensite was small, the strengthening effect of abrasion on the subsurface layer of the investigated alloys was clearly indicated by Knoop hardness measurements.

Phase study of SiO2-ZrO2 composites prepared from polymorphic combination of starting powders via a ball-milling followed by calcination

NASA Astrophysics Data System (ADS)

Musyarofah; Nurlaila, R.; Muwwaqor, N. F.; Saukani, M.; Kuswoyo, A.; Triwikantoro; Pratapa, S.

2017-04-01

The effects of SiO2-ZrO2 polymorphic combinations as starting powders and calcination temperature on phase composition of the SiO2-ZrO2 composites were studied. Stoichiometric (1:1 mol%) mixtures of the SiO2-ZrO2 composites were mechanically activated using a ball-milling for 5 h followed by calcinations at 1000, 1100 and 1200 °C for 3 h. The composites used in the present study were a-SiO2+ a-ZrO2, a-SiO2+ t-ZrO2, c-SiO2+ a-ZrO2 and c-SiO2+ t-ZrO2 which were symbolized by AA, AT, CA and CT, respectively. Prefixes a, t and c denote amorphous, tetragonal and cristobalite, respectively. The phase composition was determined by Rietveld analysis of X-ray diffraction (XRD) data using Rietica software. The identified phases for all calcined samples were a combination among t-ZrO2, c-SiO2, m-ZrO2 and zircon (ZrSiO4). Amorphous zirconia formed a transient tetragonal zirconia phase during heating, which reacted with silica to form zircon. The zircon phase was not found to form even at 1200 °C in the AT and CT mixtures and at 1100 °C in the CA mixture. The AA mixture in particular crystallized to form zircon at a lower temperature with more composition fraction than the others, ca 82.9 (14) mol%.

Unraveling the synthesis of homoleptic [Ag(N,N-diaryl-NHC)2]Y (Y = BF4, PF6) complexes by ball-milling.

PubMed

Beillard, Audrey; Bantreil, Xavier; Métro, Thomas-Xavier; Martinez, Jean; Lamaty, Frédéric

2016-11-28

A user-friendly and general mechanochemical method was developed to access rarely described NHC (N-heterocyclic carbene) silver(i) complexes featuring N,N-diarylimidazol(idin)ene ligands and non-coordinating tetrafluoroborate or hexafluorophosphate counter anions. Comparison with syntheses in solution clearly demonstrated the superiority of the ball-milling conditions.

Powder metallurgy preparation of Mg-Ca alloy for biodegradable implant application

NASA Astrophysics Data System (ADS)

Annur, D.; Suhardi, A.; Amal, M. I.; Anwar, M. S.; Kartika, I.

2017-04-01

Magnesium and its alloys is a promising candidate for implant application especially due to its biodegradability. In this study, Mg-7Ca alloys (in weight %) were processed by powder metallurgy from pure magnesium powder and calcium granule. Milling process was done in a shaker mill using stainless steel balls in various milling time (3, 5, and 8 hours) followed by compaction and sintering process. Different sintering temperatures were used (450°C and 550°C) to examine the effect of sintering temperature on mechanical properties and corrosion resistance. Microstructure evaluation was characterized by X-ray diffraction, scanning electron microscope and energy dispersive X-ray spectroscopy. Mechanical properties and corrosion behavior were examined through hardness testing and electrochemical testing in Hank’s solution (simulation body fluid). In this report, a prolonged milling time reduced particle size and later affected mechanical properties of Mg alloy. Meanwhile, the phase analysis showed that α Mg, Mg2Ca, MgO phases were formed after the sintering process. Further, this study showed that Mg-Ca alloy with different powder metallurgy process would have different corrosion rate although there were no difference of Ca content in the alloy.

Mechanically Milled Irregular Zinc Nanoparticles for Printable Bioresorbable Electronics.

PubMed

Mahajan, Bikram K; Yu, Xiaowei; Shou, Wan; Pan, Heng; Huang, Xian

2017-05-01

Bioresorbable electronics is predominantly realized by complex and time-consuming anhydrous fabrication processes. New technology explores printable methods using inks containing micro- or nano-bioresorbable particles (e.g., Zn and Mg). However, these particles have seldom been obtained in the context of bioresorbable electronics using cheap, reliable, and effective approaches with limited study on properties essential to printable electronics. Here, irregular nanocrystalline Zn with controllable sizes and optimized electrical performance is obtained through ball milling approach using polyvinylpyrrolidone (PVP) as a process control agent to stabilize Zn particles and prevent cold welding. Time and PVP dependence of the ball milled particles are studied with systematic characterizations of morphology and composition of the nanoparticles. The results reveal crystallized Zn nanoparticles with a size of ≈34.834 ± 1.76 nm and low surface oxidation. The resulting Zn nanoparticles can be readily printed onto bioresorbable substrates and sintered at room temperature using a photonic sintering approach, leading to a high conductivity of 44 643 S m -1 for printable zinc nanoparticles. The techniques to obtain Zn nanoparticles through ball milling and processing them through photonic sintering may potentially lead to a mass fabrication method for bioresorbable electronics and promote its applications in healthcare, environmental protection, and consumer electronics. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Insertion compounds and composites made by ball milling for advanced sodium-ion batteries

PubMed Central

Zhang, Biao; Dugas, Romain; Rousse, Gwenaelle; Rozier, Patrick; Abakumov, Artem M.; Tarascon, Jean-Marie

2016-01-01

Sodium-ion batteries have been considered as potential candidates for stationary energy storage because of the low cost and wide availability of Na sources. However, their future commercialization depends critically on control over the solid electrolyte interface formation, as well as the degree of sodiation at the positive electrode. Here we report an easily scalable ball milling approach, which relies on the use of metallic sodium, to prepare a variety of sodium-based alloys, insertion layered oxides and polyanionic compounds having sodium in excess such as the Na4V2(PO4)2F3 phase. The practical benefits of preparing sodium-enriched positive electrodes as reservoirs to compensate for sodium loss during solid electrolyte interphase formation are demonstrated by assembling full C/P′2-Na1[Fe0.5Mn0.5]O2 and C/‘Na3+xV2(PO4)2F3' sodium-ion cells that show substantial increases (>10%) in energy storage density. Our findings may offer electrode design principles for accelerating the development of the sodium-ion technology. PMID:26777573

Rivastigmine hydrogen tartrate polymorphs: Solid-state characterisation of transition and polymorphic conversion via milling

NASA Astrophysics Data System (ADS)

Amaro, Maria Inês; Simon, Alice; Cabral, Lúcio Mendes; de Sousa, Valéria Pereira; Healy, Anne Marie

2015-11-01

Rivastigmine (RHT) is an active pharmaceutical ingredient that is used for the treatment of mild to moderately severe dementia in Alzheimer's disease, and is known to present two polymorphic forms and to amorphise upon granulation. To date there is no information in the scientific or patent literature on polymorphic transition and stability. Hence, the aim of the current study was to gain a fundamental understanding of the polymorphic forms by (1) evaluating RHT thermodynamic stability (monotropy or enantiotropy) and (2) investigating the potential for polymorphic transformation upon milling. The two polymorphic and amorphous forms were characterised using X-ray powder diffractometry, thermal analyses, infra-red spectroscopy and water sorption analysis. The polymorphic transition was found to be spontaneous (ΔG0 < 0) and exothermic (ΔH0 < 0), indicative of a monotropic polymorph pair. The kinetic studies showed a fast initial polymorphic transition characterised by a heterogeneous nucleation, followed by a slow crystal growth. Ball milling can be used to promote the polymorphic transition and for the production of RHT amorphous form.

Effect of process control agent on the structural and magnetic properties of nano/amorphous Fe0.7Nb0.1Zr0.1Ti0.1 powders prepared by high energy ball milling

NASA Astrophysics Data System (ADS)

Khazaei Feizabad, Mohammad Hossein; Sharafi, Shahriar; Khayati, Gholam Reza; Ranjbar, Mohammad

2018-03-01

In this study, amorphous Fe0.7Nb0.1Zr0.1Ti0.1 alloy without metalloids was produced by mechanical alloying of pure mixture elements. Miedema's semi-empirical model was employed to predict the possibility of amorphous phase formation in proposed alloying system. The effect of Hexane as process control agent (PCA) on the structural, magnetic, morphological and thermal properties of the products was investigated. The results showed that the presence of PCA was necessary for the formation of amorphous phase as well as improved its soft magnetic properties. The PCA addition causes an increase of the saturation magnetization (about 43%) and decrease of the coercivity (about 50%). Moreover, the sample milled without PCA, showed a wide particle size distribution as well as relatively spherical geometry. While, in the presence of PCA the powders were aspherical and Polygon. In addition, the crystallization and Curie temperatures were found to be around 800 °C and 650 °C, respectively which are relatively high values for these kinds of alloys.

Surface modification of calcined kaolin with toluene diisocyanate based on high energy ball milling

NASA Astrophysics Data System (ADS)

Yuan, Yongbing; Chen, Hongling; Lin, Jinbin; Ji, Yan

2013-11-01

The surface of calcined kaolin particle was modified with toluene diisocyanate (TDI) by using high energy ball milling. The prepared hybrids were characterized by FT-IR, MAS NMR, thermal analysis (TGA-DSC), static water contact angle (CA), apparent viscosity and transmission electron microscopy (TEM). FT-IR and MAS NMR spectra demonstrated that TDI molecules were chemically anchored to kaolin surface after modification. The results of thermal analysis showed that the maximum grafting ratio reached up to 446.61% when the mass ratio of TDI/kaolin was 0.5:1.0, and CA measurements revealed that the resultant hybrids exhibited strong hydrophobicity (148.82°). Apparent viscosity and TEM were employed to examine the dispersion properties of blank and modified kaolin particles in poly (dimenthylsiloxane) matrix. The results illustrated that the dispersion stability depended strongly on the grafting ratio of TDI, neither too low nor too high achieved uniform and stable dispersion, and the favorable grafting ratio was obtained when the mass ratio of TDI/kaolin was 0.2:1.0. Further modification of TDI/kaolin (mass ration of TDI/kaolin, 1.0:1.0) particles with bis(aminopropyl)-terminated-poly(dimethylsiloxane) (APS) was also investigated. TEM evidenced that the dispersion properties of the obtained TDI/APS/kaolin particles were remarkably improved in octamethyl cyclotetrasiloxane compared with the original TDI/kaolin particles.

Preparation of Mo-Re-C samples containing Mo7Re13C with the β-Mn-type structure by solid state reaction of planetary-ball-milled powder mixtures of Mo, Re and C, and their crystal structures and superconductivity

NASA Astrophysics Data System (ADS)

Oh-ishi, Katsuyoshi; Nagumo, Kenta; Tateishi, Kazuya; Takafumi, Ohnishi; Yoshikane, Kenta; Sugiyama, Machiko; Oka, Kengo; Kobayashi, Ryota

2017-01-01

Mo-Re-C compounds containing Mo7Re13C with the β-Mn structure were synthesized with high-melting-temperature metals Mo, Re, and C powders using a conventional solid state method with a planetary ball milling machine instead of the arc melting method. Use of the ball milling machine was necessary to obtain Mo7Re13C with the β-Mn structure using the solid state method. Almost single-phase Mo7Re13C with a trace of impurity were obtained using the synthesis method. By XRF and lattice parameter measurements on the samples, Fe element existed in the compound synthesized using the planetary ball milling machine with a pot and balls made of steel, though Fe element was not detected in the compound synthesized using a pot and balls made of tungsten carbide. The former compound containg the Fe atom did not show superconductivity but the latter compound without the Fe atom showed superconductivity at 6.1 K.

Sharpening ball-nose mill cutters

NASA Technical Reports Server (NTRS)

Burch, C. F.

1977-01-01

Economical attachment allows faster, more precise grinding. Vibrationless and rigid relation between grinding wheel and cutter allows for extremely high finish and accurate grinding. Leveling device levels flutes with respect to toolholder rotation that generates ball-nose radius. Constant relief around entire profile of cutting edge produces longer tool life.

The influence of amorphization methods on the apparent solubility and dissolution rate of tadalafil.

PubMed

Wlodarski, K; Sawicki, W; Paluch, K J; Tajber, L; Grembecka, M; Hawelek, L; Wojnarowska, Z; Grzybowska, K; Talik, E; Paluch, M

2014-10-01

This study for the first time investigates the solubility and dissolution rate of amorphous tadalafil (Td)--a poorly water soluble chemical compound which is commonly used for treating the erectile dysfunction. To convert the crystalline form of Td drug to its amorphous counterpart we have employed most of the commercially available amorphization techniques i.e. vitrification, cryogenic grinding, ball milling, spray drying, freeze drying and antisolvent precipitation. Among the mentioned methods only quenched cooling of the molten sample was found to be an inappropriate method of Td amorphization. This is due to the thermal decomposition of Td above 200°C, as proved by the thermogravimetric analysis (TGA). Disordered character of all examined samples was confirmed using differential scanning calorimetry (DSC) and X-ray powder diffraction (PXRD). In the case of most amorphous powders, the largest 3-fold increase of apparent solubility was observed after 5 min, indicating their fast recrystallization in water. On the other hand, the partially amorphous precipitate of Td and hypromellose enhanced the solubility of Td approximately 14 times, as compared with a crystalline substance, which remained constant for half an hour. Finally, disk intrinsic dissolution rate (DIDR) of amorphous forms of Td was also examined. Copyright © 2014 Elsevier B.V. All rights reserved.

Easily recycled Bi2O3 photocatalyst coatings prepared via ball milling followed by calcination

NASA Astrophysics Data System (ADS)

Cheng, Lijun; Hu, Xumin; Hao, Liang

2017-06-01

Bi2O3 photocatalyst coatings derived from Bi coatings were first prepared by a two-step method, namely ball milling followed by the calcination process. The as-prepared samples were characterized by XRD, SEM, XPS and UV-Vis spectra, respectively. The results showed that monoclinic Bi2O3 coatings were obtained after sintering Bi coatings at 673 or 773 K, while monoclinic and triclinic mixed phase Bi2O3 coatings were obtained at 873 or 973 K. The topographies of the samples were observably different, which varied from flower-like, irregular, polygonal to nanosized particles with the increase in calcination temperature. Photodegradation of malachite green under simulated solar irradiation for 180 min showed that the largest degradation efficiency of 86.2% was achieved over Bi2O3 photocatalyst coatings sintered at 873 K. The Bi2O3 photocatalyst coatings, encapsulated with Al2O3 ball with an average diameter around 1 mm, are quite easily recycled, which provides an alternative visible light-driven photocatalyst suitable for practical water treatment application.

In-situ catalyzation approach for enhancing the hydrogenation/dehydrogenation kinetics of MgH2 powders with Ni particles

PubMed Central

El-Eskandarany, M. Sherif; Shaban, Ehab; Ali, Naser; Aldakheel, Fahad; Alkandary, Abdullah

2016-01-01

One practical solution for utilizing hydrogen in vehicles with proton-exchange fuel cells membranes is storing hydrogen in metal hydrides nanocrystalline powders. According to its high hydrogen capacity and low cost of production, magnesium hydride (MgH2) is a desired hydrogen storage system. Its slow hydrogenation/dehydrogenation kinetics and high thermal stability are the major barriers restricting its usage in real applications. Amongst the several methods used for enhancing the kinetics behaviors of MgH2 powders, mechanically milling the powders with one or more catalyst species has shown obvious advantages. Here we are proposing a new approach for gradual doping MgH2 powders with Ni particles upon ball milling the powders with Ni-balls milling media. This proposed is-situ method showed mutually beneficial for overcoming the agglomeration of catalysts and the formation of undesired Mg2NiH4 phase. Moreover, the decomposition temperature and the corresponding activation energy showed low values of 218 °C and 75 kJ/mol, respectively. The hydrogenation/dehydrogenation kinetics examined at 275 °C of the powders milled for 25 h took place within 2.5 min and 8 min, respectively. These powders containing 5.5 wt.% Ni performed 100-continuous cycle-life time of hydrogen charging/discharging at 275 °C within 56 h without failure or degradation. PMID:27849033

In-situ catalyzation approach for enhancing the hydrogenation/dehydrogenation kinetics of MgH2 powders with Ni particles

NASA Astrophysics Data System (ADS)

El-Eskandarany, M. Sherif; Shaban, Ehab; Ali, Naser; Aldakheel, Fahad; Alkandary, Abdullah

2016-11-01

One practical solution for utilizing hydrogen in vehicles with proton-exchange fuel cells membranes is storing hydrogen in metal hydrides nanocrystalline powders. According to its high hydrogen capacity and low cost of production, magnesium hydride (MgH2) is a desired hydrogen storage system. Its slow hydrogenation/dehydrogenation kinetics and high thermal stability are the major barriers restricting its usage in real applications. Amongst the several methods used for enhancing the kinetics behaviors of MgH2 powders, mechanically milling the powders with one or more catalyst species has shown obvious advantages. Here we are proposing a new approach for gradual doping MgH2 powders with Ni particles upon ball milling the powders with Ni-balls milling media. This proposed is-situ method showed mutually beneficial for overcoming the agglomeration of catalysts and the formation of undesired Mg2NiH4 phase. Moreover, the decomposition temperature and the corresponding activation energy showed low values of 218 °C and 75 kJ/mol, respectively. The hydrogenation/dehydrogenation kinetics examined at 275 °C of the powders milled for 25 h took place within 2.5 min and 8 min, respectively. These powders containing 5.5 wt.% Ni performed 100-continuous cycle-life time of hydrogen charging/discharging at 275 °C within 56 h without failure or degradation.

Carbon Nanotube-Reinforced Aluminum Matrix Composites Produced by High-Energy Ball Milling

NASA Astrophysics Data System (ADS)

Travessa, Dilermando N.; da Rocha, Geovana V. B.; Cardoso, Kátia R.; Lieblich, Marcela

2017-05-01

Although multiwall carbon nanotubes (MWCNT) are promising materials to strengthen lightweight aluminum matrix composites, their dispersion into the metallic matrix is challenge. In the present work, MWCNT were dispersed into age-hardenable AA6061 aluminum alloy by high-energy ball milling and the blend was subsequently hot-extruded. The composite bars obtained were heat-treated by solution heat treatment at 520 °C and artificially aged at 177 °C for 8 h, in order to reach the T6 temper. Special attention was given to the integrity of the MWCNT along the entire composite production. The microstructure of the obtained bars was evaluated by optical and scanning electron microscopy, and the mechanical properties were evaluated by Vickers microhardness tests. Raman spectroscopy, x-ray diffraction and transmission electron microscopy were employed to evaluate the structural integrity of MWCNT. It was found that milling time is critical to reach a proper dispersion of the reinforcing phase. The composite hardness increased up to 67% with the dispersion of 2% in weight of MWCNT, when comparing with un-reinforced bars produced by similar route. However, age hardening was not observed in composite bars after heat treatment. It was also found that MWCNT continuously degraded along the process, being partially converted into Al4C3 in the final composite.

Nitrogen-doped graphene by all-solid-state ball-milling graphite with urea as a high-power lithium ion battery anode

NASA Astrophysics Data System (ADS)

Liu, Chao; Liu, Xingang; Tan, Jiang; Wang, Qingfu; Wen, Hao; Zhang, Chuhong

2017-02-01

Nitrogen-doped graphene nanosheets (NGNS) are prepared by a novel mechanochemical method via all-solid-state ball-milling graphite with urea. The ball-milling process does not only successfully exfoliate the graphite into multi-layer (<10 layers) graphene nanosheets, but at the same time, enables the N element to be doped onto the graphene. Urea, acting as a new solid doping and assist-grinding agents, has the advantages of low cost and good water solubility that can simplify the fabrication process. The as-prepared NGNS are investigated in detail by XRD, SEM, HRTEM, TGA, XPS and Raman spectroscopy. The doping nitrogens are around 3.15% and dominated (>94%) by pyrindic-N and pyrrolic-N which facilitates the NGNS with enhanced electronic conductivity and Li-ion storage capability. For the first time, we demonstrate that the all-solid-state prepared NGNS exhibits, especially at high currents, enhanced cycling stability and rate capability as Lithium ion battery (LIB) anode active material when compared to pristine graphite and undoped graphene in half-cell configuration. The method presented in this article may provide a simple, clean, economical and scalable strategy for preparation of NGNS as a feasible and promising anode material for LIBs.

Air-stable hydrogen generation materials and enhanced hydrolysis performance of MgH2-LiNH2 composites

NASA Astrophysics Data System (ADS)

Ma, Miaolian; Ouyang, Liuzhang; Liu, Jiangwen; Wang, Hui; Shao, Huaiyu; Zhu, Min

2017-08-01

Hydrolysis of materials in water can be a promising solution of onsite hydrogen generation for realization of hydrogen economy. In this work, it was the first time that the MgH2-LiNH2 composites were explored as air-stable hydrolysis system for hydrogen generation. The MgH2-LiNH2 composites with different composition ratios were synthesized by ball milling with various durations and the hydrogen generation performances of the composite samples were investigated and compared. X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy techniques were adopted to elucidate the performance improvement mechanisms. The hydrolysis properties of MgH2 were found to be significantly enhanced by the introduction of LiNH2. The 4MgH2-LiNH2 composite ball milled for 5 h can generate 887.2 mL g-1 hydrogen in 1 min and 1016 mL g-1 in 50 min, one of the best results so far for Mg based hydrolysis materials. The LiOH·H2O and NH4OH phases of hydrolysis products from LiNH2 may prevent formation of Mg(OH)2 passivation layer on the surface and supply enough channels for hydrolysis of MgH2. The MgH2-LiNH2 composites appeared to be very stable in air and no obvious negative effect on kinetics and hydrogen generation yield was observed. These good performances demonstrate that the studied MgH2-LiNH2 composites can be a promising and practicable hydrogen generation system.

Reactive Ball Milling to Fabricate Nanocrystalline Titanium Nitride Powders and Their Subsequent Consolidation Using SPS

NASA Astrophysics Data System (ADS)

El-Eskandarany, M. Sherif

2017-05-01

The room-temperature reactive ball milling (RBM) approach was employed to synthesize nanostructured fcc-titanium nitride (TiN) powders, starting from milling hcp-titanium (Ti) powders under 10 bar of a nitrogen gas atmosphere, using a roller mill. During the first and intermediate stage of milling, the agglomerated Ti powders were continuously disintegrated into smaller particles with fresh surfaces. Increasing the RBM time led to an increase in the active-fresh surfaces of Ti, resulting increasing of the mole fraction of TiN against unreacted hcp-Ti. Toward the end of the RBM time (20 h), ultrafine spherical powder (with particles 0.5 μm in diameter) of the fcc-TiN phase was obtained, composed of nanocrystalline grains with an average diameter of 8 nm. The samples obtained after different stages of RBM time were consolidated under vacuum at 1600 °C into cylindrical bulk compacts of 20 mm diameter, using spark plasma sintering technique. These compacts that maintained their nanocrystalline characteristics with an average grain size of 56 nm in diameter, possessed high relative density (above 99% of the theoretical density). The Vickers hardness of the as-consolidated TiN was measured and found to be 22.9 GPa. The modulus of elasticity and shear modulus of bulk TiN were measured by a nondestructive test and found to be 384 and 189 GPa, respectively. In addition, the coefficient of friction of the end-product TiN bulk sample was measured and found to be 0.35.

Low Thermal Conductivity of Bulk Amorphous Si1- x Ge x Containing Nano-Sized Crystalline Particles Synthesized by Ball-Milling Process

NASA Astrophysics Data System (ADS)

Muthusamy, Omprakash; Nishino, Shunsuke; Ghodke, Swapnil; Inukai, Manabu; Sobota, Robert; Adachi, Masahiro; Kiyama, Makato; Yamamoto, Yoshiyuki; Takeuchi, Tsunehiro; Santhanakrishnan, Harish; Ikeda, Hiroya; Hayakawa, Yasuhiro

2018-06-01

Amorphous Si0.65Ge0.35 powder containing a small amount of nano-sized crystalline particles was synthesized by means of the mechanical alloying process. Hot pressing for 24 h under the pressure of 400 MPa at 823 K, which is below the crystallization temperature, allowed us to obtain bulk amorphous Si-Ge alloy containing a small amount of nanocrystals. The thermal conductivity of the prepared bulk amorphous Si-Ge alloy was extremely low, showing a magnitude of less than 1.35 Wm-1 K-1 over the entire temperature range from 300 K to 700 K. The sound velocity of longitudinal and transverse waves for the bulk amorphous Si0.65Ge0.35 were measured, and the resulting values were 5841 m/s and 2840 m/s, respectively. The estimated mean free path of phonons was kept at the very small value of ˜ 4.2 nm, which was mainly due to the strong scattering limit of phonons in association with the amorphous structure.

Comparison of particle sizes between 238PuO 2 before aqueous processing, after aqueous processing, and after ball milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mulford, Roberta Nancy

Particle sizes determined for a single lot of incoming Russian fuel and for a lot of fuel after aqueous processing are compared with particle sizes measured on fuel after ball-milling. The single samples of each type are believed to have particle size distributions typical of oxide from similar lots, as the processing of fuel lots is fairly uniform. Variation between lots is, as yet, uncharacterized. Sampling and particle size measurement methods are discussed elsewhere.

Modeling of Surface Geometric Structure State After Integratedformed Milling and Finish Burnishing

NASA Astrophysics Data System (ADS)

Berczyński, Stefan; Grochała, Daniel; Grządziel, Zenon

2017-06-01

The article deals with computer-based modeling of burnishing a surface previously milled with a spherical cutter. This method of milling leaves traces, mainly asperities caused by the cutting crossfeed and cutter diameter. The burnishing process - surface plastic treatment - is accompanied by phenomena that take place right in the burnishing ball-milled surface contact zone. The authors present the method for preparing a finite element model and the methodology of tests for the assessment of height parameters of a surface geometrical structure (SGS). In the physical model the workpieces had a cuboidal shape and these dimensions: (width × height × length) 2×1×4.5 mm. As in the process of burnishing a cuboidal workpiece is affected by plastic deformations, the nonlinearities of the milled item were taken into account. The physical model of the process assumed that the burnishing ball would be rolled perpendicularly to milling cutter linear traces. The model tests included the application of three different burnishing forces: 250 N, 500 N and 1000 N. The process modeling featured the contact and pressing of a ball into the workpiece surface till the desired force was attained, then the burnishing ball was rolled along the surface section of 2 mm, and the burnishing force was gradually reduced till the ball left the contact zone. While rolling, the burnishing ball turned by a 23° angle. The cumulative diagrams depict plastic deformations of the modeled surfaces after milling and burnishing with defined force values. The roughness of idealized milled surface was calculated for the physical model under consideration, i.e. in an elementary section between profile peaks spaced at intervals of crossfeed passes, where the milling feed fwm = 0.5 mm. Also, asperities after burnishing were calculated for the same section. The differences of the obtained values fall below 20% of mean values recorded during empirical experiments. The adopted simplification in after-milling

Synthesis of Nanostructured Carbides of Titanium and Vanadium from Metal Oxides and Ferroalloys Through High-energy Mechanical Milling and Heat Treatment

NASA Astrophysics Data System (ADS)

Basu, P.; Jian, P. F.; Seong, K. Y.; Seng, G. S.; Masrom, A. K.; Hussain, Z.; Aziz, A.

2010-03-01

Carbides of Ti and V have been synthesized directly from their oxides and ferroalloys through mechanical milling and heat treatment. The powder mixtures are milled in a planetary ball mill from 15-80 hours and subsequently heat treated at 1000-1300° C for TiO2-C mixtures, at 500-550° C for V2O5-C mixtures and at 600-1000° C for (Fe-V)-C mixtures. The milled and heat treated powders are characterized by SEM, EDAX, XRD, and BET techniques. Nanostructured TiC has been successfully synthesized under suitable processing conditions. However, carbides of vanadium is unidentified even though possibilities of V2O5-C reaction are indicated with an extent of induced amorphism in the powder mixture. Density, specific surface area and particle size of the milled and heat treated mixtures are correlated with heat treatment temperatures. Similar attempts are also made to synthesize vanadium carbides from industrial grade Fe-V.

Connecting defects and amorphization in UiO-66 and MIL-140 metal–organic frameworks: a combined experimental and computational study.

PubMed

Bennett, Thomas D; Todorova, Tanya K; Baxter, Emma F; Reid, David G; Gervais, Christel; Bueken, Bart; Van de Voorde, B; De Vos, Dirk; Keen, David A; Mellot-Draznieks, Caroline

2016-01-21

The mechanism and products of the structural collapse of the metal–organic frameworks (MOFs) UiO-66, MIL-140B and MIL-140C upon ball-milling are investigated through solid state 13C NMR and pair distribution function (PDF) studies, finding amorphization to proceed by the breaking of a fraction of metal–ligand bonding in each case. The amorphous products contain inorganic–organic bonding motifs reminiscent of the crystalline phases. Whilst the inorganic Zr6O4(OH)4 clusters of UiO-66 remain intact upon structural collapse, the ZrO backbone of the MIL-140 frameworks undergoes substantial distortion. Density functional theory calculations have been performed to investigate defective models of MIL-140B and show, through comparison of calculated and experimental 13C NMR spectra, that amorphization and defects in the materials are linked.

Investigation on hydrogenation performance of Mg{sub 2}Ni+10 wt.% NbN composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Xin; Han, Shumin; State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004

2015-01-15

The Mg{sub 2}Ni+10 wt.% NbN composite was prepared by mechanical milling and its hydrogen absorption/desorption properties and microstructure were systematically investigated. XRD results indicated that NbN was stable during ball milling process while partly decomposed into NbN{sub 0.95} and NbH during hydriding/dehydriding cycles irreversibly. The composite exhibited excellent hydrogenation/dehydrogenation kinetics performance with 2.71 wt.% hydrogen absorbed in 60 s at 423 K and 0.81 wt.% hydrogen released in 2 h at 523 K, respectively. The H diffusion constant of the composite reached 14.98×10{sup −5} s{sup −1} which was more than twice increased than that of pure Mg{sub 2}Ni powder. Themore » superior hydrogen storage properties of the composite were ascribed to the refined grain size and abundant N-defect points provided by NbN and NbN{sub 0.95} in the composite. - Graphical abstract: The Mg{sub 2}Ni+10 wt.% NbN composite displays improvements on particle size distribution as well as hydrogen storage properties compared with that of pure Mg{sub 2}Ni. - Highlights: • NbN is introduced into Mg{sub 2}Ni hydride by Ar protected ball-milling. • Surfaces of the additive NbN particle are reduced by Mg{sub 2}NiH{sub 4}. • Hydrogenation kinetic property at 423 K is double improved. • Dehydrogenation capacity at 523 K of composites is beyond double improved.« less

NORTH ELEVATION OF GOLD HILL MILL, LOOKING SOUTH. AT LEFT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

NORTH ELEVATION OF GOLD HILL MILL, LOOKING SOUTH. AT LEFT EDGE IS THE SINGLE CYLINDER “HOT SHOT” ENGINE THAT PROVIDED POWER FOR THE MILL. JUST IN FRONT OF IT IS AN ARRASTRA. AT CENTER IS THE BALL MILL AND SECONDARY ORE BIN. JUST TO THE RIGHT OF THE BALL MILL IS A RAKE CLASSIFIER, AND TO THE RIGHT ARE THE CONCENTRATION TABLES. WARM SPRINGS CAMP IS IN THE DISTANCE. SEE CA-292-4 FOR IDENTICAL B&W NEGATIVE. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

NORTH ELEVATION OF GOLD HILL MILL, LOOKING SOUTH. AT LEFT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

NORTH ELEVATION OF GOLD HILL MILL, LOOKING SOUTH. AT LEFT EDGE IS THE SINGLE CYLINDER “HOT SHOT” ENGINE THAT PROVIDED POWER FOR THE MILL. JUST IN FRONT OF IT IS AN ARRASTRA. AT CENTER IS THE BALL MILL AND SECONDARY ORE BIN. JUST TO THE RIGHT OF THE BALL MILL IS A RAKE CLASSIFIER, AND TO THE RIGHT ARE THE CONCENTRATION TABLES. WARM SPRINGS CAMP IS IN THE DISTANCE. SEE CA-292-17 (CT) FOR IDENTICAL COLOR TRANSPARENCY. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

Optical and Acoustic Sensor-Based 3D Ball Motion Estimation for Ball Sport Simulators †.

PubMed

Seo, Sang-Woo; Kim, Myunggyu; Kim, Yejin

2018-04-25

Estimation of the motion of ball-shaped objects is essential for the operation of ball sport simulators. In this paper, we propose an estimation system for 3D ball motion, including speed and angle of projection, by using acoustic vector and infrared (IR) scanning sensors. Our system is comprised of three steps to estimate a ball motion: sound-based ball firing detection, sound source localization, and IR scanning for motion analysis. First, an impulsive sound classification based on the mel-frequency cepstrum and feed-forward neural network is introduced to detect the ball launch sound. An impulsive sound source localization using a 2D microelectromechanical system (MEMS) microphones and delay-and-sum beamforming is presented to estimate the firing position. The time and position of a ball in 3D space is determined from a high-speed infrared scanning method. Our experimental results demonstrate that the estimation of ball motion based on sound allows a wider activity area than similar camera-based methods. Thus, it can be practically applied to various simulations in sports such as soccer and baseball.

Synthesis and Characterization of Al-Doped Mg2Si Thermoelectric Materials

NASA Astrophysics Data System (ADS)

Battiston, S.; Fiameni, S.; Saleemi, M.; Boldrini, S.; Famengo, A.; Agresti, F.; Stingaciu, M.; Toprak, M. S.; Fabrizio, M.; Barison, S.

2013-07-01

Magnesium silicide (Mg2Si)-based alloys are promising candidates for thermoelectric (TE) energy conversion for the middle to high range of temperature. These materials are very attractive for TE research because of the abundance of their constituent elements in the Earth's crust. Mg2Si could replace lead-based TE materials, due to its low cost, nontoxicity, and low density. In this work, the role of aluminum doping (Mg2Si:Al = 1: x for x = 0.005, 0.01, 0.02, and 0.04 molar ratio) in dense Mg2Si materials was investigated. The synthesis process was performed by planetary milling under inert atmosphere starting from commercial Mg2Si pieces and Al powder. After ball milling, the samples were sintered by means of spark plasma sintering to density >95%. The morphology, composition, and crystal structure of the samples were characterized by field-emission scanning electron microscopy, energy-dispersive spectroscopy, and x-ray diffraction analyses. Moreover, Seebeck coefficient analyses, as well as electrical and thermal conductivity measurements were performed for all samples up to 600°C. The resultant estimated ZT values are comparable to those reported in the literature for these materials. In particular, the maximum ZT achieved was 0.50 for the x = 0.01 Al-doped sample at 600°C.

Microstructure transformation of Cr-Al coating on carbon steel prepared by ball milling method as a function of tungsten doping

NASA Astrophysics Data System (ADS)

Wismogroho, A. S.; Sudiro, T.; Didik, A.; Ciswandi

2018-03-01

In present work, Cr-Al coatings containing 0, 1, 2, 3, and 5% W have been prepared on the surface of low carbon steel by mechanical alloying technique. The composition of each powder was milled for 2 hour in a stainless steel crucible with a ball to powder ratio of 10:1. Afterward, the Cr-Al-W powder and substrate were mechanically alloyed in air for 1 hour. The heat treatment of coated samples was carried out at 800 °C in a vacuum furnace for 2 hour. In order to characterize the phase composition and microstructure of the coating before and after heat treatment, XRD and SEM-EDX were used. The analysis results reveal that the ball milling process induces the formation of homogeneous Cr-Al-W coating structure with a thickness of about 80 μm. The phase observation shows individual peaks of each starting elements, along with the occurrence of powder refinement and solid solution formation. After heat treatment, AlCr2 and Al8Cr5 phases were formed. The addition of W accelerates the formation of AlCr2, but inhibits the formation of Al8Cr5. The detail of the results was presented in this paper.

Purification of Tronoh Silica Sand via preliminary process of mechanical milling

NASA Astrophysics Data System (ADS)

H, Nazratulhuda; M, Othman

2016-02-01

The purification of Tronoh silica sand is an important step in expanding technical applications of this silica sand. However no research on purifying of Tronoh silica sand has been reported. This study is focused on ball milling technique as a preliminary technique for Tronoh silica sand purification. The objectives are to study the effect of ball milling to the purification of the silica sand and to analyze its characteristics after the ball milling process. The samples before and after milling process were analyzed by using XRF, XRD, SEM and TEM. Results showed that the purity of SiO2 was increased, the size of the particles has been reduced and the surface area has increased. The crystalline phases for the silica before and after 4 hour milling time were remained constant.

Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Swain, Basudev, E-mail: swain@iae.re.kr; Mishra, Chinmayee; Kang, Leeseung

Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium,more » two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na{sub 2}CO{sub 3}, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na{sub 2}CO{sub 3}, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4 M HCl, 100 °C and pulp density of 20 g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching. - Highlights: • Simplest process for treatment of GaN an LED industry waste developed. • The process developed recovers gallium from waste LED waste dust. • Thermal analysis and phase properties of GaN to Ga{sub 2}O{sub 3} and GaN to NaGaO{sub 2} revealed. • Solid-state chemistry involved in this process reported. • Quantitative leaching of the GaN was achieved.« less

Phase transformation and magnetic properties of MnAl powders prepared by elemental-doping and salt-assisted ball milling

NASA Astrophysics Data System (ADS)

Qian, Hui-Dong; Si, Ping-Zhan; Choi, Chul-Jin; Park, Jihoon; Cho, Kyung Mox

2018-05-01

The effects of elemental doping of Si and Fe on the ɛ→τ phase transformation and the magnetic properties of MnAl were studied. The magnetic powders of Si- and Fe-doped MnAl were prepared by using induction melting followed by water-quenching, annealing, and salt-assisted ball-milling. The Fe-doped MnAl powders are mainly composed of the L10-structured τ-phase, while the Si-doped MnAl are composed of τ-phase and a small fraction of γ2- and β-phases. A unique thin leaves-like morphology with thickness of several tens of nanometers and diameter size up to 500 nm were observed in the Si-doped MnAl powders. The Fe-doped MnAl powders show irregular shape with much larger dimensions in the range from several to 10 μm. The morphology difference of the samples was ascribed to the variation of the mechanical properties affected by different doping elements. The phase transformation temperatures of the ɛ-phase of the samples were measured. The doping of Fe decreases the onset temperature of the massive phase transformation in MnAl, while the Si-doping increases the massive phase transformation temperature. Both Fe and Si increase the Curie temperature of MnAl. A substantially enhanced coercivity up to 0.45 T and 0.42 T were observed in the ball-milled MnAl powders doped with Si and Fe, respectively.

Preparation of Zn(BH4)2 and diborane and hydrogen release properties of Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15)

NASA Astrophysics Data System (ADS)

Kwak, Young Jun; Kwon, Sung Nam; Song, Myoung Youp

2015-09-01

Zn(BH4)2 was prepared by milling ZnCl2 and NaBH4 in a planetary ball mill under Ar atmosphere, and Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15) samples were prepared. Diborane (B2H6) and hydrogen release characteristics of the Zn(BH4)2 and Zn(BH4)2+xMgH2 samples were studied. The samples synthesized by milling ZnCl2 and NaBH4 contained Zn(BH4)2 and NaCl, together with small amounts of ZnCl2 and NaBH4. We designated these samples as Zn(BH4)2(+NaCl). The weight loss up to 400 °C of the Zn(BH4)2(+NaCl) sample synthesized by milling 4 h was 11.2 wt%. FT-IR analysis showed that Zn(BH4)2 was formed in the Zn(BH4)2(+NaCl) samples. MgH2 was also milled in a planetary ball mill, and mixed with the Zn(BH4)2(+NaCl) synthesized by milling for 4 h in a mortar and pestle. The weight loss up to 400 °C of Zn(BH4)2(+NaCl)+MgH2 was 8.2 wt%, corresponding to the weight % of diborane and hydrogen released from the Zn(BH4)2(+NaCl)+MgH2 sample, with respect to the sample weight. DTA results of Zn(BH4)2(+NaCl)+xMgH2 showed that the decomposition peak of Zn(BH4)2 was at about 61 °C, and that of MgH2 was at about 370-389 °C.

A Fundamental Approach to Developing Aluminium based Bulk Amorphous Alloys based on Stable Liquid Metal Structures and Electronic Equilibrium - 154041

DTIC Science & Technology

2017-03-28

AFRL-AFOSR-JP-TR-2017-0027 A Fundamental Approach to Developing Aluminium-based Bulk Amorphous Alloys based on Stable Liquid -Metal Structures and...to 16 Dec 2016 4.  TITLE AND SUBTITLE A Fundamental Approach to Developing Aluminium-based Bulk Amorphous Alloys based on Stable Liquid -Metal...including Al, Cu, Ni, Zr, Mg, Pd, Ga , Ca. Many new Al-based amorphous alloys were found within the numerous alloy systems studied in this project, and

Morphology and magnetic properties of CeCo5 submicron flakes prepared by surfactant-assisted high-energy ball milling

NASA Astrophysics Data System (ADS)

Zhang, J. J.; Gao, H. M.; Yan, Y.; Bai, X.; Su, F.; Wang, W. Q.; Du, X. B.

2012-10-01

CeCo5 permanent magnetic alloy has been processed by surfactant assisted high energy ball milling. Heptane and oleic acid were used as the solvent and surfactant, respectively. The amount of surfactant used was 50% by weight of the starting powder. The produced particles were deposited on a piece of copper (4 mm in length and width) under a magnetic field of 27 kOe applied along the copper surface and immobilized by ethyl α-cyanoacrylate. Scanning electron microscope pictures show that the particles are flakes, several μm in length and width and tens of nm in thickness. X-ray diffraction patterns and magnetic measurements prove that the flakes are crystalline with c-axes magnetic anisotropy. The easy magnetization axis is oriented perpendicular to the surface of the flake. A maximum coercivity of 3.3 kOe was obtained for the sample milled for 40 min.

Magnetism of Amorphous and Nano-Crystallized Dc-Sputter-Deposited MgO Thin Films

PubMed Central

Mahadeva, Sreekanth K.; Fan, Jincheng; Biswas, Anis; Sreelatha, K.S.; Belova, Lyubov; Rao, K.V.

2013-01-01

We report a systematic study of room-temperature ferromagnetism (RTFM) in pristine MgO thin films in their amorphous and nano-crystalline states. The as deposited dc-sputtered films of pristine MgO on Si substrates using a metallic Mg target in an O2 containing working gas atmosphere of (N2 + O2) are found to be X-ray amorphous. All these films obtained with oxygen partial pressure (PO2) ~10% to 80% while maintaining the same total pressure of the working gas are found to be ferromagnetic at room temperature. The room temperature saturation magnetization (MS) value of 2.68 emu/cm3 obtained for the MgO film deposited in PO2 of 10% increases to 9.62 emu/cm3 for film deposited at PO2 of 40%. However, the MS values decrease steadily for further increase of oxygen partial pressure during deposition. On thermal annealing at temperatures in the range 600 to 800 °C, the films become nanocrystalline and as the crystallite size grows with longer annealing times and higher temperature, MS decreases. Our study clearly points out that it is possible to tailor the magnetic properties of thin films of MgO. The room temperature ferromagnetism in MgO films is attributed to the presence of Mg cation vacancies. PMID:28348346

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

Hot Melt Extrusion and Spray Drying of Co-amorphous Indomethacin-Arginine With Polymers.

PubMed

Lenz, Elisabeth; Löbmann, Korbinian; Rades, Thomas; Knop, Klaus; Kleinebudde, Peter

2017-01-01

Co-amorphous drug-amino acid systems have gained growing interest as an alternative to common amorphous formulations which contain polymers as stabilizers. Several preparation methods have recently been investigated, including vibrational ball milling on a laboratory scale or spray drying in a larger scale. In this study, the feasibility of hot melt extrusion for continuous manufacturing of co-amorphous drug-amino acid formulations was examined, challenging the fact that amino acids melt with degradation at high temperatures. Furthermore, the need for an addition of a polymer in this process was evaluated. After a polymer screening via the solvent evaporation method, co-amorphous indomethacin-arginine was prepared by a melting-solvent extrusion process without and with copovidone. The obtained products were characterized with respect to their solid-state properties, non-sink dissolution behavior, and stability. Results were compared to those of spray-dried formulations with the same compositions and to spray-dried indomethacin-copovidone. Overall, stable co-amorphous systems could be prepared by extrusion without or with copovidone, which exhibited comparable molecular interaction properties to the respective spray-dried products, while phase separation was detected by differential scanning calorimetry in several cases. The formulations containing indomethacin in combination with arginine and copovidone showed enhanced dissolution behavior over the formulations with only copovidone or arginine. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Toughening Fe-based Amorphous Coatings by Reinforcement of Amorphous Carbon.

PubMed

Wang, Wei; Zhang, Cheng; Zhang, Zhi-Wei; Li, Yi-Cheng; Yasir, Muhammad; Wang, Hai-Tao; Liu, Lin

2017-06-22

Toughening of Fe-based amorphous coatings meanwhile maintaining a good corrosion resistance remains challenging. This work reports a novel approach to improve the toughness of a FeCrMoCBY amorphous coating through in-situ formation of amorphous carbon reinforcement without reducing the corrosion resistance. The Fe-based composite coating was prepared by high velocity oxy-fuel (HVOF) thermal spraying using a pre-mixed Fe-based amorphous/nylon-11 polymer feedstock powders. The nylon-11 powders were in-situ carbonized to amorphous carbon phase during thermal spraying process, which homogeneously distributed in the amorphous matrix leading to significant enhancement of toughness of the coating. The mechanical properties, including hardness, impact resistance, bending and fatigue strength, were extensively studied by using a series of mechanical testing techniques. The results revealed that the composite coating reinforced by amorphous carbon phase exhibited enhanced impact resistance and nearly twice-higher fatigue strength than that of the monolithic amorphous coating. The enhancement of impact toughness and fatigue properties is owed to the dumping effect of the soft amorphous carbon phase, which alleviated stress concentration and decreased crack propagation driving force.

Drawing Sensors with Ball-Milled Blends of Metal-Organic Frameworks and Graphite

PubMed Central

Ko, Michael; Aykanat, Aylin; Smith, Merry K.

2017-01-01

The synthetically tunable properties and intrinsic porosity of conductive metal-organic frameworks (MOFs) make them promising materials for transducing selective interactions with gaseous analytes in an electrically addressable platform. Consequently, conductive MOFs are valuable functional materials with high potential utility in chemical detection. The implementation of these materials, however, is limited by the available methods for device incorporation due to their poor solubility and moderate electrical conductivity. This manuscript describes a straightforward method for the integration of moderately conductive MOFs into chemiresistive sensors by mechanical abrasion. To improve electrical contacts, blends of MOFs with graphite were generated using a solvent-free ball-milling procedure. While most bulk powders of pure conductive MOFs were difficult to integrate into devices directly via mechanical abrasion, the compressed solid-state MOF/graphite blends were easily abraded onto the surface of paper substrates equipped with gold electrodes to generate functional sensors. This method was used to prepare an array of chemiresistors, from four conductive MOFs, capable of detecting and differentiating NH3, H2S and NO at parts-per-million concentrations. PMID:28946624

H 2 Desorption from MgH 2 Surfaces with Steps and Catalyst-Dopants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reich, Jason M.; Wang, Lin-Lin; Johnson, Duane D.

2014-03-10

Light-metal hydrides, like MgH 2, remain under scrutiny as prototypes for reversible H-storage materials. For MgH 2, we assess hydrogen desorption/adsorption properties (enthalpy and kinetic barriers) for stepped, catalyst-doped surfaces occurring, e.g., from ball-milling in real samples. Employing density functional theory and simulated annealing in a slab model, we studied initial H 2 desorption from stepped surfaces with(out) titanium (Ti) catalytic dopant. Extensive simulated annealing studies were performed to find the dopant’s site preferences. For the most stable initial and final (possibly magnetic) states, nudged elastic band (NEB) calculations were performed to determine the H 2-desorption activation energy. We usedmore » a moment-transition NEB method to account for the dopant’s transition to the lowest-energy magnetic state at each image along the band. We identify a dopant-related surface-desorption mechanism that reloads via bulk H diffusion. While reproducing the observed bulk enthalpy of desorption, we find a decrease of 0.24 eV (a 14% reduction) in the activation energy on doped stepped surface; together with a 22% reduction on a doped flat surface, this brackets the assessed 18% reduction in kinetic barrier for ball-milled MgH 2 samples with low concentration of Ti from experiment.« less

Effect of ball milling and dynamic compaction on magnetic properties of Al2O3/Co(P) composite particles

NASA Astrophysics Data System (ADS)

Denisova, E. A.; Kuzovnikova, L. A.; Iskhakov, R. S.; Bukaemskiy, A. A.; Eremin, E. V.; Nemtsev, I. V.

2014-05-01

The evolution of the magnetic properties of composite Al2O3/Co(P) particles during ball milling and dynamic compaction is investigated. To prepare starting composite particles, the Al2O3 granules were coated with a Co95P5 shell by electroless plating. The magnetic and structural properties of the composite particles are characterized by scanning electron microscopy, X-ray diffraction, and the use of the Physical Property Measurement System. The use of composite core-shell particles as starting powder for mechanoactivation allows to decrease treatment duration to 1 h and to produce a more homogeneous bulk sample than in the case of the mixture of Co and Al2O3 powders. The magnetic properties of the milled composite particles are correlated with changes in the microstructure. Reduction in grain size of Co during milling leads to an increase of the volume fraction of superparamagnetic particles and to a decrease of the saturation magnetization. The local magnetic anisotropy field depends on the amount of hcp-Co phase in sample. The anisotropy field value decreases from 8.4 kOe to 3.8 kOe with an increase in milling duration up to 75 min. The regimes of dynamic compaction were selected so that the magnetic characteristics—saturation magnetization and coercive field—remained unchanged.

Effective utilizations of palm oil mill fly ash for synthetic amorphous silica and carbon zeolite composite synthesis

NASA Astrophysics Data System (ADS)

Utama, P. S.; Saputra, E.; Khairat

2018-04-01

Palm Oil Mill Fly Ash (POMFA) the solid waste of palm oil industry was used as a raw material for synthetic amorphous silica and carbon zeolite composite synthesis in order to minimize the wastes of palm oil industry. The alkaline extraction combine with the sol-gel precipitation and mechanical fragmentation was applied to produce synthetic amorphous silica. The byproduct, extracted POMFA was rich in carbon and silica content in a significant amount. The microwave heated hydrothermal process used to synthesize carbon zeolite composite from the byproduct. The obtained silica had chemical composition, specific surface area and the micrograph similar to commercial precipitated silica for rubber filler. The microwave heated hydrothermal process has a great potential for synthesizing carbon zeolite composite. The process only needs one-step and shorter time compare to conventional hydrothermal process.

Combining hot-compressed water and ball milling pretreatments to improve the efficiency of the enzymatic hydrolysis of eucalyptus

PubMed Central

Inoue, Hiroyuki; Yano, Shinichi; Endo, Takashi; Sakaki, Tsuyoshi; Sawayama, Shigeki

2008-01-01

Background Lignocellulosic biomass such as wood is an attractive material for fuel ethanol production. Pretreatment technologies that increase the digestibility of cellulose and hemicellulose in the lignocellulosic biomass have a major influence on the cost of the subsequent enzymatic hydrolysis and ethanol fermentation processes. Pretreatments without chemicals such as acids, bases or organic solvents are less effective for an enzymatic hydrolysis process than those with chemicals, but they have a less negative effect on the environment. Results The enzymatic digestibility of eucalyptus was examined following a combined pretreatment without chemicals comprising a ball milling (BM) and hot-compressed water (HCW) treatment. The BM treatment simultaneously improved the digestibility of both glucan and xylan, and was effective in lowering the enzyme loading compared with the HCW treatment. The combination of HCW and BM treatment reduced the BM time. The eucalyptus treated with HCW (160°C, 30 minutes) followed by BM (20 minutes) had an approximately 70% yield of total sugar with a cellulase loading of 4 FPU/g substrate. This yield was comparable to the yields from samples treated with HCW (200°C, 30 minutes) or BM (40 minutes) hydrolyzed with 40 FPU/g substrate. Conclusion The HCW treatment is useful in improving the milling efficiency. The combined HCW-BM treatment can save energy and enzyme loading. PMID:18471309

Lignocellulose fermentation and residual solids characterization for senescent switchgrass fermentation by Clostridium thermocellum in the presence and absence of continuous in situ ball-milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balch, Michael L.; Holwerda, Evert K.; Davis, Mark F.

Milling during lignocellulosic fermentation, henceforth referred to as cotreatment, is investigated as an alternative to thermochemical pretreatment as a means of enhancing biological solubilization of lignocellulose. We investigate the impact of milling on soluble substrate fermentation by Clostridium thermocellum with comparison to yeast, document solubilization for fermentation of senescent switchgrass with and without ball milling, and characterize residual solids. Soluble substrate fermentation by C. thermocellum proceeded readily in the presence of continuous ball milling but was completely arrested for yeast. Total fractional carbohydrate solubilization achieved after fermentation of senescent switchgrass by C. thermocellum for 5 days was 0.45 without cotreatmentmore » or pretreatment, 0.81 with hydrothermal pretreatment (200 degrees C, 15 minutes, severity 4.2), and 0.88 with cotreatment. Acetate and ethanol were the main fermentation products, and were produced at similar ratios with and without cotreatment. Analysis of solid residues was undertaken using molecular beam mass spectrometry (PyMBMS) and solid-state nuclear magnetic resonance spectroscopy (NMR) in order to provide insight into changes in plant cell walls during processing via various modes. The structure of lignin present in residual solids remaining after fermentation with cotreatment appeared to change little, with substantially greater changes observed for hydrothermal pretreatment - particularly with respect to formation of C-C bonds. The observation of high solubilization with little apparent modification of the residue is consistent with cotreatment enhancing solubilization primarily by increasing the access of saccharolytic enzymes to the feedstock, and C. thermocellum being able to attack all the major linkages in cellulosic biomass provided that these linkages are accessible.« less

Determination of ethyl glucuronide in hair: a rapid sample pretreatment involving simultaneous milling and extraction.

PubMed

Mönch, Bettina; Becker, Roland; Nehls, Irene

2014-01-01

A combination of simultaneous milling and extraction known as micropulverized extraction was developed for the quantification of the alcohol marker ethyl glucuronide (EtG) in hair samples using a homogeneous reference material and a mixer mill. Best extraction results from 50 mg of hair were obtained with 2-mL plastic tubes containing two steel balls (∅ = 5 mm), 0.5 mL of water and with an oscillating frequency of 30 s(-1) over a period of 30 min. EtG was quantified employing a validated GC-MS procedure involving derivatization with pentafluoropropionic acid anhydride. This micropulverization procedure was compared with dry milling followed by separate aqueous extraction and with aqueous extraction after manual cutting to millimeter-size snippets. Micropulverization yielded 28.0 ± 1.70 pg/mg and was seen to be superior to manually cutting (23.0 ± 0.83 pg/mg) and equivalent to dry grinding (27.7 ± 1.71 pg/mg) with regard to completeness of EtG extraction. The option to process up to 20 samples simultaneously makes micropulverization especially valuable for the high throughput of urgent samples.

The milling of pristine and brominated P-100 graphite fibers

NASA Technical Reports Server (NTRS)

Dillehay, M. E.; Gaier, J. R.

1986-01-01

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.

Preparation of Mo-Re-C samples containing Mo{sub 7}Re{sub 13}C with the β-Mn-type structure by solid state reaction of planetary-ball-milled powder mixtures of Mo, Re and C, and their crystal structures and superconductivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oh-ishi, Katsuyoshi, E-mail: oh-ishi@kc.chuo-u.ac.jp; Nagumo, Kenta; Tateishi, Kazuya

Mo-Re-C compounds containing Mo{sub 7}Re{sub 13}C with the β-Mn structure were synthesized with high-melting-temperature metals Mo, Re, and C powders using a conventional solid state method with a planetary ball milling machine instead of the arc melting method. Use of the ball milling machine was necessary to obtain Mo{sub 7}Re{sub 13}C with the β-Mn structure using the solid state method. Almost single-phase Mo{sub 7}Re{sub 13}C with a trace of impurity were obtained using the synthesis method. By XRF and lattice parameter measurements on the samples, Fe element existed in the compound synthesized using the planetary ball milling machine with amore » pot and balls made of steel, though Fe element was not detected in the compound synthesized using a pot and balls made of tungsten carbide. The former compound containg the Fe atom did not show superconductivity but the latter compound without the Fe atom showed superconductivity at 6.1 K. - Graphical abstract: Temperature dependence of the magnetic susceptibility measured under 10 Oe for the superconducting PBM-T samples without Fe element and non-superconducting PBM-S with Fe element. The inset is the enlarged view of the data for the PBM-S sample.« less

Bulk superhard B-C-N nanocomposite compact and method for preparing thereof

DOEpatents

Zhao, Yusheng; He, Duanwei

2004-07-06

Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

Superthermostability of nanoscale TIC-reinforced copper alloys manufactured by a two-step ball-milling process

NASA Astrophysics Data System (ADS)

Wang, Fenglin; Li, Yunping; Xu, Xiandong; Koizumi, Yuichiro; Yamanaka, Kenta; Bian, Huakang; Chiba, Akihiko

2015-12-01

A Cu-TiC alloy, with nanoscale TiC particles highly dispersed in the submicron-grained Cu matrix, was manufactured by a self-developed two-step ball-milling process on Cu, Ti and C powders. The thermostability of the composite was evaluated by high-temperature isothermal annealing treatments, with temperatures ranging from 727 to 1273 K. The semicoherent nanoscale TiC particles with Cu matrix, mainly located along the grain boundaries, were found to exhibit the promising trait of blocking grain boundary migrations, which leads to a super-stabilized microstructures up to approximately the melting point of copper (1223 K). Furthermore, the Cu-TiC alloys after annealing at 1323 K showed a slight decrease in Vickers hardness as well as the duplex microstructure due to selective grain growth, which were discussed in terms of hardness contributions from various mechanisms.

Fabrication of superconducting nanowires from ultrathin MgB2 films via focused ion beam milling

NASA Astrophysics Data System (ADS)

Zhang, Chen; Wang, Da; Liu, Zheng-Hao; Zhang, Yan; Ma, Ping; Feng, Qing-Rong; Wang, Yue; Gan, Zi-Zhao

2015-02-01

High quality superconducting nanowires were fabricated from ultrathin MgB2 films by a focused ion beam milling technique. The precursor MgB2 films in 10 nm thick were grown on MgO substrates by using a hybrid physical-chemical vapor deposition method. The nanowires, in widths of about 300-600 nm and lengths of 1 or 10 μm, showed high superconducting critical temperatures (Tc's) above 34 K and narrow superconducting transition widths (ΔTc's) of 1-3 K. The superconducting critical current density Jc of the nanowires was above 5 × 107 A/cm2 at 20 K. The high Tc, narrow ΔTc, and high Jc of the nanowires offered the possibility of making MgB2-based nano-devices such as hot-electron bolometers and superconducting nanowire single-photon detectors with high operating temperatures at 15-20 K.

N-type nano-silicon powders with ultra-low electrical resistivity as anode materials in lithium ion batteries

NASA Astrophysics Data System (ADS)

Yue, Zhihao; Zhou, Lang; Jin, Chenxin; Xu, Guojun; Liu, Liekai; Tang, Hao; Li, Xiaomin; Sun, Fugen; Huang, Haibin; Yuan, Jiren

2017-06-01

N-type silicon wafers with electrical resistivity of 0.001 Ω cm were ball-milled to powders and part of them was further mechanically crushed by sand-milling to smaller particles of nano-size. Both the sand-milled and ball-milled silicon powders were, respectively, mixed with graphite powder (silicon:graphite = 5:95, weight ratio) as anode materials for lithium ion batteries. Electrochemical measurements, including cycle and rate tests, present that anode using sand-milled silicon powder performed much better. The first discharge capacity of sand-milled silicon anode is 549.7 mAh/g and it is still up to 420.4 mAh/g after 100 cycles. Besides, the D50 of sand-milled silicon powder shows ten times smaller in particle size than that of ball-milled silicon powder, and they are 276 nm and 2.6 μm, respectively. In addition, there exist some amorphous silicon components in the sand-milled silicon powder excepting the multi-crystalline silicon, which is very different from the ball-milled silicon powder made up of multi-crystalline silicon only.

Magnetic properties of FeCuNbSiB nanocrystalline alloy powder cores using ball-milled powder

NASA Astrophysics Data System (ADS)

Kim, G. H.; Noh, T. H.; Choi, G. B.; Kim, K. Y.

2003-05-01

Cold-pressed nanocrystalline powder cores were fabricated using powders of nanocrystalline ribbons which were ball milled for short time. Their magnetic properties at high frequency were measured. The powder size ranges from 20 to 850 μm and the contents of the glass binder are between 1 and 8 wt %. For cores composed of large particles of 300-850 μm with 5 wt % glass binder, we obtained a stable permeability of 100 up to 800 kHz, a maximum level 31 of quality factor at frequency of 50 kHz, and 320 mW/cm3 core loss at f=50 kHz and Bm=0.1 T. This is mainly due to the good soft magnetic properties of the powders and the higher insulation of powder cores which cause low eddy current losses.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

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 ballmore » 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.« less

Amino acids as co-amorphous stabilizers for poorly water soluble drugs--Part 1: preparation, stability and dissolution enhancement.

PubMed

Löbmann, Korbinian; Grohganz, Holger; Laitinen, Riikka; Strachan, Clare; Rades, Thomas

2013-11-01

Poor aqueous solubility of an active pharmaceutical ingredient (API) is one of the most pressing problems in pharmaceutical research and development because up to 90% of new API candidates under development are poorly water soluble. These drugs usually have a low and variable oral bioavailability, and therefore an unsatisfactory therapeutic effect. One of the most promising approaches to increase dissolution rate and solubility of these drugs is the conversion of a crystalline form of the drug into its respective amorphous form, usually by incorporation into hydrophilic polymers, forming glass solutions. However, this strategy only led to a small number of marketed products usually because of inadequate physical stability of the drug (crystallization). In this study, we investigated a fundamentally different approach to stabilize the amorphous form of drugs, namely the use of amino acids as small molecular weight excipients that form specific molecular interactions with the drug resulting in co-amorphous forms. The two poorly water soluble drugs carbamazepine and indomethacin were combined with amino acids from the binding sites of the biological receptors of these drugs. Mixtures of drug and the amino acids arginine, phenylalanine, tryptophan and tyrosine were prepared by vibrational ball milling. Solid-state characterization with X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC) revealed that the various blends could be prepared as homogeneous, single phase co-amorphous formulations indicated by the appearance of an amorphous halo in the XRPD diffractograms and a single glass transition temperature (Tg) in the DSC measurements. In addition, the Tgs of the co-amorphous mixtures were significantly increased over those of the individual drugs. The drugs remained chemically stable during the milling process and the co-amorphous formulations were generally physically stable over at least 6 months at 40 °C under dry conditions. The

Properties of dispersion-strengthened chromium - 4-volume-percent-thoria alloys produced by ball milling in hydrogen iodide

NASA Technical Reports Server (NTRS)

Arias, A.

1974-01-01

The effects of processing variables on the tensile properties and ductile-to-brittle transition temperature (DBTT) of Cr + 4 vol. %ThO2 alloys and of pure Cr produced by ball milling in hydrogen iodide were investigated. Hot rolled Cr + ThO2 was stronger than either hot pressed Cr + ThO2 or pure Cr at temperatures up to 1537 C. Hot pressed Cr + ThO2 had a DBTT of 501 C as compared with minus 8 to 24 C for the hot rolled Cr + ThO2 and with 139 C for pure Cr. It is postulated that the dispersoid in the hot rolled alloys lowers the DBTT by inhibiting recovery and recrystallization of the strained structure.

Role of chemical interaction between MgH2 and TiO2 additive on the hydrogen storage behavior of MgH2

NASA Astrophysics Data System (ADS)

Pukazhselvan, D.; Nasani, Narendar; Sandhya, K. S.; Singh, Budhendra; Bdikin, Igor; Koga, Nobuaki; Fagg, Duncan Paul

2017-10-01

The present study explores how the additive titania chemically reacts with magnesium hydride and influences the dehydrogenation of MgH2. Quantitative X - ray diffraction study of ball milled MgH2 + xTiO2 (x = 0.25, 0.33, 0.5 and 1) suggests that Ti substituted MgO is the main reaction product in all the product powders. Convincing evidence is obtained to conclude that Ti dissolution in MgO makes a dramatic behavioral change to MgO; passive MgO turns as an active in-built catalyst. The analysis correlating the dehydrogenation kinetics, composition of in-situ catalyst and sample durability suggests that effectiveness of Ti substituted MgO (MgxTiyOx+y) as a catalyst for MgH2 depends on the concentration of Ti in MgxTiyOx+y rock salt. These observations are immensely helpful for understanding the hydrogen desorption mechanism of metal oxide additives loaded MgH2 system.

Particle size reduction of Si3N4 with Si3N4 milling hardware

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Freedman, M. R.; Kiser, J. D.

1986-01-01

The grinding of Si3N4 powder using reaction bonded Si3N4 attrition, vibratory, and ball mills with Si3N4 media was examined. The rate of particle size reduction and the change in the chemical composition of the powder were determined in order to compare the grinding efficiency and the increase in impurity content resulting from mill and media wear for each technique. Attrition and vibratory milling exhibited rates of specific surface area increase that were approximately eight times that observed in ball milling. Vibratory milling introduced the greatest impurity pickup.

Magneto-optical properties of α-Fe2O3@ZnO nanocomposites prepared by the high energy ball-milling technique

NASA Astrophysics Data System (ADS)

Chaudhury, Chandana Roy; Roychowdhury, Anirban; Das, Anusree; Das, Dipankar

2016-05-01

Magnetic-fluorescent nanocomposites (NCs) with 10 wt% of α-Fe2O3 in ZnO have been prepared by the high energy ball-milling. The crystallite sizes of α-Fe2O3 and ZnO in the NCs are found to vary from 65 nm to 20 nm and 47 nm to 15 nm respectively as milling time is increased from 2 to 30 h. XRD analysis confirms presence of α-Fe2O3 and ZnO in pure form in all the NCs. UV-vis study of the NCs shows a continuous blue-shift of the absorption peak and a steady increase of band gap of ZnO with increasing milling duration that are assigned to decreasing particle size of ZnO in the NCs. Photoluminescence (PL) spectra of the NCs reveal three weak emission bands in the visible region at 421, 445 and 485 nm along with the strong near band edge emission at 391 nm. These weak emission bands are attributed to different defect - related energy levels e.g. Zn-vacancy, Zn interstitial and oxygen vacancy. Dc and ac magnetization measurements show presence of weakly interacting superparamagnetic (SPM) α-Fe2O3 particles in the NCs. 57Fe-Mössbauer study confirms presence of SPM hematite in the sample milled for 30 h. Positron annihilation lifetime measurements indicate presence of cation vacancies in ZnO nanostructures confirming results of PL studies.

DEM modeling of ball mills with experimental validation: influence of contact parameters on charge motion and power draw

NASA Astrophysics Data System (ADS)

Boemer, Dominik; Ponthot, Jean-Philippe

2017-01-01

Discrete element method simulations of a 1:5-scale laboratory ball mill are presented in this paper to study the influence of the contact parameters on the charge motion and the power draw. The position density limit is introduced as an efficient mathematical tool to describe and to compare the macroscopic charge motion in different scenarios, i.a. with different values of the contact parameters. While the charge motion and the power draw are relatively insensitive to the stiffness and the damping coefficient of the linear spring-slider-damper contact law, the coefficient of friction has a strong influence since it controls the sliding propensity of the charge. Based on the experimental calibration and validation by charge motion photographs and power draw measurements, the descriptive and predictive capabilities of the position density limit and the discrete element method are demonstrated, i.e. the real position of the charge is precisely delimited by the respective position density limit and the power draw can be predicted with an accuracy of about 5 %.

Fabrication of nanocrystalline surface composite layer on Cu plate under ball collisions.

PubMed

Romankov, S; Park, Y C; Yoon, J M

2014-10-01

It was demonstrated that the severe plastic deformation of a surface induced by repeated ball collisions can be effectively used for fabrication of the nanocrystalline surface composite layers. The Cu disk was fixed at the top of a vibration chamber and ball treated. Al, Zr, Ni, Co and Fe were introduced into a Cu plate as contaminants from the grinding media one after the other by 15-min ball treatment. The composite structure was formed as a result of mechanical intermixing of the components. The particle size in as-fabricated layer ranged from 2 nm to 20 nm, with average values of about 7 nm. As-fabricated layer contained non-equilibrium multicomponent solid solution based on FCC Cu crystal structure, Zr-based phase, nanosized steel debris and amorphous phase. The hardness of the as-fabricated composite was almost ten times that of the initial Cu plate.

Mechanical and Microstructure Study of Nickel-Based ODS Alloys Processed by Mechano-Chemical Bonding and Ball Milling

NASA Astrophysics Data System (ADS)

Amare, Belachew N.

Due to the need to increase the efficiency of modern power plants, land-based gas turbines are designed to operate at high temperature creating harsh environments for structural materials. The elevated turbine inlet temperature directly affects the materials at the hottest sections, which includes combustion chamber, blades, and vanes. Therefore, the hottest sections should satisfy a number of material requirements such as high creep strength, ductility at low temperature, high temperature oxidation and corrosion resistance. Such requirements are nowadays satisfied by implementing superalloys coated by high temperature thermal barrier coating (TBC) systems to protect from high operating temperature required to obtain an increased efficiency. Oxide dispersive strengthened (ODS) alloys are being considered due to their high temperature creep strength, good oxidation and corrosion resistance for high temperature applications in advanced power plants. These alloys operating at high temperature are subjected to different loading systems such as thermal, mechanical, and thermo-mechanical combined loads at operation. Thus, it is critical to study the high temperature mechanical and microstructure properties of such alloys for their structural integrity. The primary objective of this research work is to investigate the mechanical and microstructure properties of nickel-based ODS alloys produced by combined mechano-chemical bonding (MCB) and ball milling subjected to high temperature oxidation, which are expected to be applied for high temperature turbine coating with micro-channel cooling system. Stiffness response and microstructure evaluation of such alloy systems was studied along with their oxidation mechanism and structural integrity through thermal cyclic exposure. Another objective is to analyze the heat transfer of ODS alloy coatings with micro-channel cooling system using finite element analysis (FEA) to determine their feasibility as a stand-alone structural

Particle-size reduction of Si3N4 powder with Si3N4 milling hardware

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Freedman, M. R.; Kiser, J. D.

1986-01-01

The grinding of Si3N4 powder using reaction bonded Si3N4 attrition, vibratory, and ball mills with Si3N4 media was examined. The rate of particle size reduction and the change in the chemical composition of the powder were determined in order to compare the grinding efficiency and the increase in impurity content resulting from mill and media wear for each technique. Attrition and vibratory milling exhibited rates of specific surface area increase that were approximately eight times that observed in ball milling. Vibratory milling introduced the greatest impurity pickup.

A comparison of amorphous calcium carbonate crystallization in aqueous solutions of MgCl2 and MgSO4: implications for paleo-ocean chemistry

NASA Astrophysics Data System (ADS)

Han, Mei; Zhao, Yanyang; Zhao, Hui; Han, Zuozhen; Yan, Huaxiao; Sun, Bin; Meng, Ruirui; Zhuang, Dingxiang; Li, Dan; Liu, Binwei

2018-04-01

Based on the terminology of "aragonite seas" and "calcite seas", whether different Mg sources could affect the mineralogy of carbonate sediments at the same Mg/Ca ratio was explored, which was expected to provide a qualitative assessment of the chemistry of the paleo-ocean. In this work, amorphous calcium carbonate (ACC) was prepared by direct precipitation in anhydrous ethanol and used as a precursor to study crystallization processes in MgSO4 and MgCl2 solutions having different concentrations at 60 °C (reaction times 240 and 2880 min). Based on the morphology of the aragonite crystals, as well as mineral saturation indices and kinetic analysis of geochemical processes, it was found that these crystals formed with a spherulitic texture in 4 steps. First, ACC crystallized into columnar Mg calcite by nearly oriented attachment. Second, the Mg calcite changed from columnar shapes into smooth dumbbell forms. Third, the Mg calcite transformed into rough dumbbell or cauliflower-shaped aragonite forms by local dissolution and precipitation. Finally, the aragonite transformed further into spherulitic radial and irregular aggregate forms. The increase in Ca2+ in the MgSO4 solutions compared with the MgCl2 solutions indicates the fast dissolution and slow precipitation of ACC in the former solutions. The phase transition was more complete in the 0.005 M MgCl2 solution, whereas Mg calcite crystallized from the 0.005 M MgSO4 solution, indicating that Mg calcite could be formed more easily in an MgSO4 solution. Based on these findings, aragonite and Mg calcite relative to ACC could be used to provide a qualitative assessment of the chemistry of the paleo-ocean. Therefore, calcite seas relative to high-Mg calcite could reflect a low concentration MgSO4 paleo-ocean, while aragonite seas could be related to an MgCl2 or high concentration of MgSO4 paleo-ocean.

The synergistic effects of combining the high energy mechanical milling and wet milling on Si negative electrode materials for lithium ion battery

NASA Astrophysics Data System (ADS)

Hou, Shang-Chieh; Su, Yuh-Fan; Chang, Chia-Chin; Hu, Chih-Wei; Chen, Tsan-Yao; Yang, Shun-Min; Huang, Jow-Lay

2017-05-01

The submicro-sized and nanostructured Si aggregated powder is prepared by combinational routes of high energy mechanical milling (HEMM) and wet milling. Milled Si powder is investigated by particle size analyzer, SEM, TEM, XPS and XRD as well as the control ones. Its electrode is also investigated by in situ XRD and electrochemical performance. Morphology reveals that combining the high energy mechanical milling and wet milling not only fracture primary Si particles but also form submicro-sized Si aggregates constructed by amorphous and nanocrystalline phases. Moreover, XPS shows that wet milling in ethanol trigger Sisbnd Osbnd CH2CH3 bonding on Si surface might enhance the SEI formation. In situ XRD analysis shows negative electrode made of submicro-sized Si aggregated powder can effectively suppress formation of crystalline Li15Si4 during lithiation and delithiation due to amorphous and nanocrystalline construction. Thus, the submicro-sized Si powder with synergistic effects combining the high energy mechanical milling and wet milling in ethanol as negative electrode performs better capacity retention.

Preparation of bulk superhard B-C-N nanocomposite compact

DOEpatents

Zhao, Yusheng [Los Alamos, NM; He, Duanwei [Sichuan, CN

2011-05-10

Bulk, superhard, B--C--N nanocomposite compacts were prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture at a pressure in a range of from about 15 GPa to about 25 GPa, and sintering the pressurized encapsulated ball-milled mixture at a temperature in a range of from about 1800-2500 K. The product bulk, superhard, nanocomposite compacts were well sintered compacts with nanocrystalline grains of at least one high-pressure phase of B--C--N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compacts had a measured Vicker's hardness in a range of from about 41 GPa to about 68 GPa.

Diamond-silicon carbide composite

DOEpatents

Qian, Jiang; Zhao, Yusheng

2006-06-13

Fully dense, diamond-silicon carbide composites are prepared from ball-milled microcrystalline diamond/amorphous silicon powder mixture. The ball-milled powder is sintered (P=5–8 GPa, T=1400K–2300K) to form composites having high fracture toughness. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPa.dot.m^1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness. X-ray diffraction patterns and Raman spectra indicate that amorphous silicon is partially transformed into nanocrystalline silicon at 5 GPa/873K, and nanocrystalline silicon carbide forms at higher temperatures.

Diamond-Silicon Carbide Composite And Method For Preparation Thereof

DOEpatents

Qian, Jiang; Zhao, Yusheng

2005-09-06

Fully dense, diamond-silicon carbide composites are prepared from ball-milled microcrystalline diamond/amorphous silicon powder mixture. The ball-milled powder is sintered (P=5-8 GPa, T=1400K-2300K) to form composites having high fracture toughness. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPa.multidot.m.sup.1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness. X-ray diffraction patterns and Raman spectra indicate that amorphous silicon is partially transformed into nanocrystalline silicon at 5 GPa/873K, and nanocrystalline silicon carbide forms at higher temperatures.

Radiation-induced amorphization of Ce-doped Mg2Y8(SiO4)6O2 silicate apatite

NASA Astrophysics Data System (ADS)

Zhou, Jianren; Yao, Tiankai; Lian, Jie; Shen, Yiqiang; Dong, Zhili; Lu, Fengyuan

2016-07-01

Ce-doped Mg2Y8(SiO4)6O2 silicate apatite (Ce = 0.05 and 0.5) were irradiated with 1 MeV Kr2+ ion beam irradiation at different temperatures and their radiation response and the cation composition dependence of the radiation-induced amorphization were studied by in situ TEM. The two Ce-doped Mg2Y8(SiO4)6O2 silicate apatites are sensitive to ion beam induced amorphization with a low critical dose (0.096 dpa) at room temperature, and exhibits significantly different radiation tolerance at elevated temperatures. Ce concentration at the apatite AI site plays a critical role in determining the radiation response of this silicate apatite, in which the Ce3+ rich Mg2Y7.5Ce0.5(SiO4)6O2 displays lower amorphization susceptibility than Mg2Y7.95Ce0.05(SiO4)6O2 with a lower Ce3+ occupancy at the AI sites. The critical temperature (Tc) and activation energy (Ea) change from 667.5 ± 33 K and 0.162 eV of Mg2Y7.5Ce0.5(SiO4)6O2 to 963.6 ± 64 K and 0.206 eV of Mg2Y7.95Ce0.05(SiO4)6O2. We demonstrate that the radiation tolerance can be controlled by varying the chemical composition, and enhanced radiation tolerance is achieved by increasing the Ce concentration at the AI site.

Dependence of rates of breakage on fines content in wet ball mill grinding

NASA Astrophysics Data System (ADS)

Bhattacharyya, Anirban

The following research fundamentally deals with the cause and implications of nonlinearities in breakage rates of materials in wet grinding systems. The innate dependence of such nonlinearities on fines content and the milling environment during wet grinding operations is also tested and observed. Preferential breakage of coarser size fractions as compared to the finer size fractions in a particle population were observed and discussed. The classification action of the pulp was deemed to be the probable cause for such a peculiarity. Ores with varying degrees of hardness and brittleness were used for wet grinding experiments, primarily to test the variations in specific breakage rates as a function of varying hardness. For this research, limestone, quartzite, and gold ore were used. The degree of hardness is of the order of: limestone, quartzite, gold ore. Selection and breakage function parameters were determined in the course of this research. Functional forms of these expressions were used to compare experimentally derived parameter estimates. Force-fitting of parameters was not done in order to examine the realtime behavior of particle populations in wet grinding systems. Breakage functions were established as being invariant with respect to such operating variables like ball load, mill speed, particle load, and particle size distribution of the mill. It was also determined that specific selection functions were inherently dependent on the particle size distribution in wet grinding systems. Also, they were consistent with inputs of specific energy, according to grind time. Nonlinearity trends were observed for 1st order specific selection functions which illustrated variations in breakage rates with incremental inputs of grind time and specific energy. A mean particle size called the fulcrum was noted below which the nonlinearities in the breakage trends were observed. This magnitude of the fulcrum value varied with percent solids and slurry filling, indicating

Enhanced hydrogen generation by hydrolysis of Mg doped with flower-like MoS2 for fuel cell applications

NASA Astrophysics Data System (ADS)

Huang, Minghong; Ouyang, Liuzhang; Liu, Jiangwen; Wang, Hui; Shao, Huaiyu; Zhu, Min

2017-10-01

In this work, flower-like MoS2 spheres are synthesized via a hydrothermal method and the catalytic activity of the as-prepared and bulk MoS2 on hydrolysis of Mg is systematically investigated for the first time. The Mg-MoS2 composites are prepared by ball milling and the hydrogen generation performances of the composites are investigated in 3.5% NaCl solution. The experimental results suggest that the as-prepared MoS2 exhibits better catalytic effect on hydrolysis of Mg compared to bulk MoS2. In particular, Mg-10 wt% MoS2 (as-prepared) composite milled for 1 h shows the best hydrogen generation properties and releases 90.4% of theoretical hydrogen generation capacity within 1 min at room temperature. The excellent catalytic effect of as-prepared MoS2 may be attributed to the following aspects: three-dimensional flower-like MoS2 architectures improve its dispersibility on Mg particles; make the composite more reactive; hamper the generated Mg(OH)2 from adhering to the surface of Mg; and increase the galvanic corrosion of Mg. In addition, a hydrogen generator based on the hydrolysis reaction of Mg-0.2 wt% MoS2 composite is manufactured and it can supply a maximum hydrogen flow rate of 2.5 L/min. The findings here demonstrate the as-prepared flower-like MoS2 can be a promising catalyst for hydrogen generation from Mg.

Surface functionalized amorphous nanosilica and microsilica with nanopores as promising tools in biomedicine

NASA Astrophysics Data System (ADS)

Rahman, Ayesha; Seth, Dipankar; Mukhopadhyaya, Sunit K.; Brahmachary, Ratan L.; Ulrichs, Christian; Goswami, Arunava

2009-01-01

Cellular interactions with engineered nanoparticles (NPs) are dependent on many properties, inherent to the nanoparticle (viz. size, shape, surface characteristics, degradation, agglomeration/dispersal, and charge, etc.). Modification of the surface reactivity via surface functionalization of the nanoparticles to be targeted seems to be important. Utilization of different surface functionalization methods of nanoparticles is an emerging field of basic and applied nanotechnology. It is well known that many disease-causing organisms induce host lipids and if deprived, their growth is inhibited in vivo. Amorphous nanosilica (ANS) and amorphous microsilica with nanopores (AMS) were prepared by a combination of wet chemistry and high-energy ball milling. Lipophilic moieties were attached to both ANS and AMS via chemical surface functionalization method. Lipophilic ANS and AMS were found to inhibit the growth of Bombyx mori nuclear polyhedrosis virus (BmNPV) and chicken malarial parasites via absorption of silkworm hemolymph and chicken serum lipids/lipoproteins, respectively, in vivo. Therefore, intelligent surface functionalization of NP is an important concept, and its application in curing chicken malaria and BmNPV is presented here. Surface functionalization method reported in this paper might serve as a valuable technology for treating many diseases where pathogens induce host lipid.

Effect of milling on the plastic and the elastic stiffness of lactose particles.

PubMed

Pazesh, Samaneh; Persson, Ann-Sofie; Berggren, Jonas; Alderborn, Göran

2018-03-01

The purpose of this study was to investigate the effect of degree of disorder of a series of α-lactose monohydrate powders, prepared by milling for different time periods, on the plastic and the elastic stiffness of the particles. As references, a series of physical mixtures consisting of original crystalline particles and amorphous particles obtained by spray-drying was used. In addition, the effect of powder pre-storage humidity on the mechanical properties was investigated. For milled particles of a low degree of disorder, a decreased particle size increased the particle plastic stiffness. For milled particles of constant particle size, the plastic stiffness decreased with an increased degree of disorder while the elastic stiffness seemed nearly independent of the degree of disorder. The presence of moisture caused a recrystallisation of milled particles with low degree of disorder which increased their plastic stiffness. For the physical mixtures of crystalline and amorphous particles, similar relationships between plastic stiffness and amorphous content as for the milled powders were obtained. A reasonable explanation is that the nature of the milled particles is represented by a two-state system with crystalline and amorphous domains. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Analysis of Particle Distribution in Milled Al-Based Composites Reinforced by B4C Nanoparticles

NASA Astrophysics Data System (ADS)

Alihosseini, Hamid; Dehghani, Kamran

2017-04-01

In the present work, high-energy ball milling was employed to synthesize Al-(5-10 wt.%)B4C nanocomposite. To do this, two sizes of particles of 50 nm as nanoparticles (NPs) and 50 μm as coarse particles (CPs) were used. The morphology and microstructure of the milled powders were characterized using particle size analyzer, SEM, TEM and EDX techniques. It was found that milling time, B4C particles size and their content strongly affect the characteristics of powders during milling process. The breaking and cold welding of powders was recognized as two main competitive actions during the milling process that influence the microstructural evolutions. It was found that the presence of CPs led to the formation of microcracks which promote the fracture process of Al powders. The dominated mechanisms during the fabrication of composites and nanocomposites were discussed. Also, the theoretical issues regarding the changes in morphology and distribution of B4C particles in CPs and NPs are clarified.

Synthesis and hydriding properties of Li 2Mg(NH) 2

NASA Astrophysics Data System (ADS)

Markmaitree, Tippawan; Shaw, Leon L.

The phase pure Li 2Mg(NH) 2 has been synthesized via a dehydriding treatment of a ball milled 2LiNH 2 + MgH 2 mixture. This phase pure Li 2Mg(NH) 2 has been utilized to investigate its hydriding kinetics at the temperature range 180-220 °C. It is found that the hydriding process of Li 2Mg(NH) 2 is very sluggish even though it has favorable thermodynamic properties for near the ambient temperature operation. Holding at 200 °C for 10 h only results in 3.75 wt.% H 2 uptake. The detailed kinetic analysis reveals that the hydriding process of Li 2Mg(NH) 2 is diffusion-controlled. Thus, this study unambiguously indicates that the future direction to enhance the hydriding kinetics of this promising hydrogen storage material system should be to minimize the diffusion distance and increase the diffusion rate.

Solvent-free MALDI-MS for the analysis of a membrane protein via the mini ball mill approach: case study of bacteriorhodopsin.

PubMed

Trimpin, Sarah; Deinzer, Max L

2007-01-01

A mini ball mill (MBM) solvent-free matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) method allows for the analysis of bacteriorhodopsin (BR), an integral membrane protein that previously presented special analytical problems. For well-defined signals in the molecular ion region of the analytes, a desalting procedure of the MBM sample directly on the MALDI target plate was used to reduce adduction by sodium and other cations that are normally attendant with hydrophobic peptides and proteins as a result of the sample preparation procedure. Mass analysis of the intact hydrophobic protein and the few hydrophobic and hydrophilic tryptic peptides available in the digest is demonstrated with this robust new approach. MS and MS/MS spectra of BR tryptic peptides and intact protein were generally superior to the traditional solvent-based method using the desalted "dry" MALDI preparation procedure. The solvent-free method expands the range of peptides that can be effectively analyzed by MALDI-MS to those that are hydrophobic and solubility-limited.

Interfacial Reaction During High Energy Ball Milling Dispersion of Carbon Nanotubes into Ti6Al4V

NASA Astrophysics Data System (ADS)

Adegbenjo, A. O.; Olubambi, P. A.; Potgieter, J. H.; Nsiah-Baafi, E.; Shongwe, M. B.

2017-12-01

The unique thermal and mechanical properties of carbon nanotubes (CNTs) have made them choice reinforcements for metal matrix composites (MMCs). However, there still remains a critical challenge in achieving homogeneous dispersion of CNTs in metallic matrices. Although high energy ball milling (HEBM) has been reported as an effective method of dispersing CNTs into metal matrices, a careful selection of the milling parameters is important not to compromise the structural integrity of CNTs which may cause interfacial reactions with the matrix. In this study, multi-walled carbon nanotubes (MWCNTs) were purified by annealing in argon and vacuum atmospheres at 1000 and 1800 °C, respectively, for 5 h to remove possible metallic catalyst impurities. Subsequently, 1, 2 and 3 wt.% MWCNTs were dispersed by adapted HEBM into Ti6Al4V alloy metal matrix. Raman spectroscopy (RS), x-ray diffraction, scanning electron microscopy, energy-dispersive x-ray spectrometry and transmission electron microscopy techniques were used to characterize the as-received and annealed MWCNTs, as well as the admixed MWCNT/Ti6Al4V nanocomposite powders. The experimental results showed that vacuum annealing successfully eliminated retained nickel (Ni) catalysts from MWCNTs, while the adapted HEBM method achieved a relative homogeneous dispersion of MWCNTs into the Ti6Al4V matrix and helped to control interfacial reactions between defective MWCNTs and the metal matrix.

New FCC Mg–Zr and Mg–Zr–ti deuterides obtained by reactive milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guzik, Matylda N., E-mail: matylda.guzik@ife.no; Deledda, Stefano; Sørby, Magnus H.

2015-03-15

Results for binary Mg–Zr and ternary Mg–Zr–Ti mixtures ball milled at room temperature under reactive deuterium atmosphere (5.6–6.7 MPa) are reported. X-ray and neutron powder diffraction combined with Rietveld refinements show that two new cubic phases were formed during milling. Mg{sub 0.40}Zr{sub 0.60}D{sub 1.78} and Mg{sub 0.40}Zr{sub 0.26}Ti{sub 0.34}D{sub 1.98} crystallize with disordered face centered cubic metal atom arrangements. Results of differential scanning calorimetry and termogravimetric measurements demonstrate that both deuterides desorb deuterium at lower temperatures than MgD{sub 2}, ZrD{sub 2} or TiD{sub 2}; 528 and 575 K in the Mg–Zr–D and Mg–Zr–Ti–D system, respectively. Interestingly, Mg{sub 0.40}Zr{sub 0.26}Ti{sub 0.34}D{submore » 1.98} stores deuterium reversibly at 673 K and 10 MPa of D{sub 2}. - Graphical abstract: High resolution SR-PXD patterns obtained for Mg{sub 0.40}Zr{sub 0.60}D{sub 1.78} and first time reported Mg{sub 0.40}Zr{sub 0.26}Ti{sub 0.34}D{sub 1.98}. - Highlights: • Synthesis and characterization of Mg{sub 0.40}Zr{sub 0.60}D{sub 1.78} and Mg{sub 0.40}Zr{sub 0.26}Ti{sub 0.34}D{sub 1.98}. • New deuterides obtained by milling under H{sub 2} gas pressure in the order of a few MPa. • Phases desorb deuterium at temperature lower than corresponding binary deuterides. • Mg{sub 0.40}Zr{sub 0.26}Ti{sub 0.34}D{sub 1.98} stores hydrogen reversibly at 673 K and 10 MPa of D{sub 2}.« less

Effect of grain size on structural and dielectric properties of barium titanate piezoceramics synthesized by high energy ball milling

NASA Astrophysics Data System (ADS)

Verma, Narendra Kumar; Patel, Sandeep Kumar Singh; Kumar, Dinesh; Singh, Chandra Bhal; Singh, Akhilesh Kumar

2018-05-01

We have investigated the effect of sintering temperature on the densification behaviour, grain size, structural and dielectric properties of BaTiO3 ceramics, prepared by high energy ball milling method. The Powder x-ray diffraction reveals the tetragonal structure with space group P4mm for all the samples. The samples were sintered at four different temperatures, (T = 900°C, 1000°C, 1100°C, 1200°C and 1300°C). Density increased with increasing sintering temperature, reaching up to 97% at 1300°C. A grain growth was observed with increasing sintering temperature. Impedance analyses of the sintered samples at various temperatures were performed. Increase in dielectric constant and Curie temperature is observed with increasing sintering temperature.

Agile Thermal Management STT-RX. Catalytic Influence of Ni-based Additives on the Dehydrogentation Properties of Ball Milled MgH2 (PREPRINT)

DTIC Science & Technology

2011-12-01

Wronski: Particle size, grain size and gamma-MgH2 effects on the desorption properties of nanocrystal- line commercial magnesium hydride processed...Catalytic effects of various forms of nickel on the synthesis rate and hydrogen desorption properties of nanocrystalline magnesium hydride (MgH2...dehydrogenation reaction. 15. SUBJECT TERMS magnesium hydride , MgH, thermal energy storage materials, endothermic reaction 16. SECURITY CLASSIFICATION

Comparison of mechanical and friction properties of composite materials based on AlMg2 containing nano-dimensional particles of crystalline graphite and nanofibers of gamma oxide of aluminum

NASA Astrophysics Data System (ADS)

Aborkin, A. V.; Babin, D. M.; Soboĺkov, A. V.

2018-04-01

The method of mechanical synthesis in a planetary ball mill was used for production of composite powders based on the AlMg2 alloy containing 1 wt. % of nanosized particles of crystalline graphite or γ-Al2O3. The resulting powders are consolidated by the sintering under pressure. Using the methods of X-ray diffraction analysis, scanning and transmission electron microscopy, the structural-phase composition of bulk composite materials was studied. Comparative analysis of the microhardness, the conditional yield stress at compression, and the friction coefficient of bulk composite materials is carried out. It has been found out that the mechanical properties of composites reinforced with γ-Al2O3 nanofibers are higher than when reinforcing with nanoscale particles of crystalline graphite.

In vitro metal ion release and biocompatibility of amorphous Mg67Zn28Ca5 alloy with/without gelatin coating.

PubMed

Chan, W Y; Chian, K S; Tan, M J

2013-12-01

Amorphous zinc-rich Mg-Zn-Ca alloys have exhibited good tissue compatibility and low hydrogen evolution in vivo. However, suboptimal cell-surface interaction on magnesium alloy surface observed in vitro could lead to reduced integration with host tissue for regenerative purpose. This study aims to improve cell-surface interaction of amorphous Mg67Zn28Ca5 alloy by coating a gelatin layer by electrospinning. Coated/uncoated alloys were immersed and extracted for 3 days under different CO2. The immersion results showed that pH and metal ion release in the alloy extracts were affected by gelatin coating and CO2, suggesting their roles in alloy biocorrosion and a mechanism has been proposed for the alloy-CO2 system with/without coating. Cytotoxicity results are evident that gelatin-coated alloy with 2-day crosslinking not only exhibited no indirect cytotoxicity, but also supported attachment of L929 and MG63 cell lines around/on the alloy with high viability. Therefore, amorphous Mg67Zn28Ca5 alloy coated with gelatin by electrospinning technique provides a useful method to improve alloy biocompatibility. © 2013 Elsevier B.V. All rights reserved.

Synthesis of ZnO Nanocrystal-Graphene Composite by Mechanical Milling and Sonication-Assisted Exfoliation

NASA Astrophysics Data System (ADS)

Arora, Sweety; Srivastava, Chandan

2017-02-01

A ZnO nanocrystal-graphene composite was synthesized by a two-step method involving mechanical milling and sonication-assisted exfoliation. Zn metal powder was first ball-milled with graphite powder for 30 h in water medium. This ball-milled mixture was then subjected to exfoliation by sonication in the presence of sodium lauryl sulfate surfactant to produce graphene decorated with spherical agglomerates of ultrafine nanocrystalline ZnO. The presence of a few layers of graphene was confirmed by Raman spectroscopy and atomic force microscopy measurements. The size, phase identity and composition of the ZnO nanocrystals was determined by transmission electron microscopy measurements.

Atmospheric Tar Balls: Particles from Biomass and Biofuel Burning

NASA Technical Reports Server (NTRS)

Posfai, Mihaly; Gelencser, Andras; Simonics, Renata; Arato, Krisztina; Li, Jia; Hobbs, Peter V.; Buseck, Peter R.

2004-01-01

Tar balls are amorphous, carbonaceous spherules that occur in the tropospheric aerosol as a result of biomass and biofuel burning. They form a distinct group of particles with diameters typically between 30 and 500 nm and readily identifiable with electron microscopy. Their lack of a turbostratic microstructure distinguishes them from soot, and their morphology and composition (approximately 90 mol% carbon) renders them distinct from other carbonaceous particles. Tar balls are particularly abundant in slightly aged (minutes to hours old) biomass smoke, indicating that they likely form by gas-to-particle conversion within smoke plumes. The material of tar balls is initially hygroscopic; however, the particles become largely insoluble as a result of free radical polymerization of their organic molecules. Consequently, tar balls are primarily externally mixed with other particle types, and they do not appreciably increase in size during aging. When tar balls coagulate with water-bearing particles, their material may partly dissolve and no longer be recognizable as distinct particles. Tar balls may contain organic compounds that absorb sunlight. They are an important, previously unrecognized type of carbonaceous (organic) atmospheric particle.

Effect of charcoal doping on the superconducting properties of MgB 2 bulk

NASA Astrophysics Data System (ADS)

Kim, N. K.; Tan, K. S.; Jun, B.-H.; Park, H. W.; Joo, J.; Kim, C.-J.

2008-09-01

The effect of charcoal doping on the superconducting properties of in situ processed MgB 2 bulk samples was investigated. To understand the size effect of the dopant the charcoal powder was attrition milled for 1 h, 3 h and 6 h using ZrO 2 balls. The milled charcoal powders were mixed with magnesium and boron powders to a nominal composition of Mg(B 0.975C 0.025) 2. The Mg(B 0.975C 0.025) 2 compacts were heat-treated at 900 °C for 0.5 h in flowing Ar atmosphere. Magnetic susceptibility for the samples showed that the superconducting transition temperature ( Tc) decreased as the size of the charcoal powder decreased. The critical current density ( Jc) of Mg(B 0.975C 0.025) 2 prepared using large size charcoal powder was lower than that of the undoped MgB 2. However, a crossover of Jc value was observed at high magnetic fields of about 4 T in Mg(B 0.975C 0.025) 2 prepared using small size charcoal powder. Carbon diffusion into the boron site was easier and gave the Jc increase effect when the small size charcoal was used as a dopant.

Milling assisted synthesis of calcium zirconate СаZrО3

NASA Astrophysics Data System (ADS)

Kalinkin, A. M.; Nevedomskii, V. N.; Kalinkina, E. V.; Balyakin, K. V.

2014-08-01

Monophase calcium zirconate (CaZrO3) has been prepared from the equimolar ZrO2 + CaCO3 mixture by two-step synthesis process. In the first step, mechanical treatment of the mixture is performed in an AGO-2 planetary ball mill. In the second step, the milled mixture is annealed to form calcium zirconate. High-energy ball milling of the (ZrO2+CaCO3) mixture results in decrease in the temperature of CaZrO3 formation during annealing at 950 °C. The enhancement of CaZrO3 synthesis is due to accumulation of excess energy by the reagents, decreasing the particle size and notable increase in the interphase area because of “smearing” of CaCO3 on ZrO2 particles during milling. Nanocrystalline calcium zirconate has been produced by controlling the annealing temperature and time.

Textured Pr{sub 2}Fe{sub 14}B flakes with submicron or nanosize thickness prepared by surfactant-assisted ball milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zuo, Wen-Liang, E-mail: wlzuo@iphy.ac.cn, E-mail: shenbg@aphy.iphy.ac.cn; Liu, Rong-Ming; Zheng, Xin-Qi

2014-05-07

The textured Pr{sub 2}Fe{sub 14}B nanoflakes were produced by surfactant-assisted ball milling (SABM). Single phase tetragonal structure was characterized for the samples before and after SABM by X-ray diffraction (XRD). The thickness and length of the as-milled flakes are mainly in the range of 50–150 nm and 0.5–2 μm, respectively. For the field-aligned Pr{sub 2}Fe{sub 14}B nanoflakes, the out-of-plane texture (the easy magnetization direction (EMD) along the c-axis) is indicated from the increasing (00l) peaks in the XRD patterns. SEM image demonstrates that the EMD is parallel to flaky surface, which is different from the RCo{sub 5} (R = rare earth) system with EMDmore » perpendicular to the surface. We propose a hypothesis that the easy glide planes are related with the area of crystal planes. In addition, a large coercivity H{sub c} = 3.9 kOe is observed in the Pr{sub 2}Fe{sub 14}B flakes with strong texture.« less

Synthesis, characterization and performance of high energy ball milled meso-scale zero valent iron in Fenton reaction.

PubMed

Ambika, Selvaraj; Devasena, M; Nambi, Indumathi Manivannan

2016-10-01

Understanding contaminant degradation by different sized zero valent iron (ZVI) particles is one important aspect in addressing the long-term stability of these particles in field studies. In this study, meso zero valent iron (mZVI) particles were synthesised in a milling time of 10 h using ball milling technique. The efficacy of mZVI particles for removal of phenol was quantitatively evaluated in comparison with coarse zero valent iron (cZVI) and nano zero valent iron (nZVI) particles. Phenol degradation experiments were carried out in sacrificial batch mode at room temperature independently with cZVI, nZVI and mZVI under varied pH conditions of 3, 4, 6, 7, 8 and 10. Batch experiments substantiating the reactivity of mZVI under unbuffered pH system were also carried out and compared with buffered and poorly buffered pH systems. mZVI particles showed consistent phenol degradation at circum-neutral pH with efficiency of 44%, 67%, and 89% in a span of 5, 10 and 20 min respectively. The dissolved iron species and residual iron formation were also measured as a function of pH. Unbuffered systems at circum-neutral pH produced less residual iron when compared to buffered and poorly buffered systems. At this pH, oxidation of Fe(2+) produced a different oxidant Ferryl ion, which was found to effectively participate in phenol degradation. Copyright © 2016 Elsevier Ltd. All rights reserved.

8. RW Meyer Sugar Mill: 18761889. Simple, singlecylinder, horizontal, reciprocating ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

8. RW Meyer Sugar Mill: 1876-1889. Simple, single-cylinder, horizontal, reciprocating steam engine, model No. 1, 5' x 10', 6 hp, 175 rpm. Manufactured by Ames Iron Works, Oswego, New York, 1879. View: Steam engine powered the mill's centrifugals. It received steam from the locomotive type, fire-tube portable boiler in the background. The engine's water pump which pumped water from the feed-water clarifying cistern, in between the boiler and engine, through a pre-heat system and on to the boiler, is seen in front of the fluted cylinder. The fly-ball governor, missing its balls, the steam port, and manual throttle valve are above and behind the cylinder. The flywheel, drive shaft, and pulley are on the left side of the engine bed. - R. W. Meyer Sugar Mill, State Route 47, Kualapuu, Maui County, HI

Effect of mechanical milling on barium titanate (BaTiO3) perovskite

NASA Astrophysics Data System (ADS)

Singh, Rajan Kumar; Sanodia, Sagar; Jain, Neha; Kumar, Ranveer

2018-05-01

Commercial Barium Titanate BaTiO3 (BT) is milled by planetary ball mill in acetone medium using stainless steel bowl & ball for different hours. BT is an important perovskite oxide with structure ABO3. BT has applications in electro-optic devices, energy storing devices such as photovoltaic cells, thermistors, multiceramic capacitors & DRAMs etc. BT is non-toxic & environment friendly ceramic with high dielectric and piezoelectric property so it can be used as the substitute of PZT & PbTiO3. Here, we have investigated the effect of milling time and temperature on particle size and phase transition of BT powder. We used use Raman spectroscopy for studying the spectra of BT; XRD is used for structural study. Intensity (height) of Raman spectra and XRD spectra continuously decrease with increasing the milling hours and width if these spectra increases which indicates, decrease in BT size.

Ultra-hard amorphous AlMgB14 films RF sputtered onto curved substrates

NASA Astrophysics Data System (ADS)

Grishin, A. M.; Putrolaynen, V. V.; Yuzvyuk, M. H.

2017-03-01

Recently, hard AlMgB14 (BAM) coatings were deposited for the first time by RF magnetron sputtering using a single stoichiometric ceramic target. High target sputtering power and sufficiently short target-to-substrate distance were found to be critical processing conditions. They enabled fabrication of stoichiometric in-depth compositionally homogeneous films with the peak values of nanohardness 88 GPa and Young’s modulus 517 GPa at the penetration depth of 26 nm and, respectively, 35 GPa and 275 GPa at 200 nm depth in 2 µm thick film (Grishin et al 2014 JETP Lett. 100 680). The narrow range of sufficiently short target-to-substrate distance makes impossible to coat non flat specimens. To achieve ultimate BAM films’ characteristics onto curved surfaces we developed two-step sputtering process. The first thin layer is deposited as a template at low RF power that facilitates a layered Frank van der Merwe mode growth of smooth film occurs. The next layer is grown at high RF target sputtering power. The affinity of subsequent flow of sputtered atoms to already evenly condensed template fosters the development of smooth film surface. As an example, we made BAM coating onto hemispherical 5 mm in diameter ball made from a hard tool steel and used as a head of a special gauge. Very smooth (6.6 nm RMS surface roughness) and hard AlMgB14 films fabricated onto commercial ball-shaped items enhance hardness of tool steel specimens by a factor of four.

Preparation of folic acid conjugated hematite nanoparticles using high energy ball milling for biomedical applications

NASA Astrophysics Data System (ADS)

Sahu, Dwipak Prasad; Jammalamadaka, S. Narayana

2018-04-01

The controlled release and targeted delivery of drug to tumour sites using magnetic nanoparticles (MNPs) for the treatment of cancer & other ailments is current focus of research. Here we describe our efforts in functionalization of hematite nanoparticles α-Fe2O3 with polyethylene glycol (PEG) and activation with Folic Acid (FA) (ligand) using a high energy ball milling process. An extra peak at 48.3° in XRD hints an encapsulation of polyethylene glycol on α-Fe2O3 nanoparticles (NPs). The decrease in the intensity of absorption spectra peaks in UV - Vis NIR spectrum pertinent to activated α-Fe2O3 NPs indicate indeed there is a conjugation of folic acid on top of PEG. Thermo-gravimetric analysis shows 5% weight loss for the activated α-Fe2O3 NPs due to desorption of chemi-adsorbed PEG from NPs and its further decomposition. Magnetization measurements indicates indeed the coercivity persists even after activating the NPs with FA. We believe presence of coercivity in MNPs can be exploited in magnetic hyperthermia treatment of cancer cell by applying suitable amount of field at the targeted site.

21. RW Meyer Sugar Mill: 18761889. Simple, singlecylinder, horizontal, reciprocating ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

21. RW Meyer Sugar Mill: 1876-1889. Simple, single-cylinder, horizontal, reciprocating steam engine, model no. 1, 5' x 10', 6 hp, 175 rpm. Manufactured by Ames Iron Works, Oswego, New York, 1879. View: Steam engine powered the mill's centrifugals. Steam-feed pipe at top left of engine. Steam exhaust pipe leaves base of engine on right end and projects upwards. The boiler feed and supply pipe running water through the engine's pre-heat system are seen running to the lower left end of the engine. Pulley in the foreground was not used. The centrifugals were powered by a belt running from the flywheel in the background. Ball-type governor and pulley are on left end of the engine. - R. W. Meyer Sugar Mill, State Route 47, Kualapuu, Maui County, HI

Fabrication of Fe1.1Se0.5Te0.5 bulk by a high energy ball milling technique

NASA Astrophysics Data System (ADS)

Liu, Jixing; Li, Chengshan; Zhang, Shengnan; Feng, Jianqing; Zhang, Pingxiang; Zhou, Lian

2017-11-01

Fe1.1Se0.5Te0.5 superconducting bulks were successfully synthesized by a high energy ball milling (HEBM) aided sintering technique. Two advantages of this new technique have been revealed compared with traditional solid state sintering method. One is greatly increased the density of sintered bulks. It is because the precursor powders with β-Fe(Se, Te) and δ-Fe(Se, Te) were obtained directly by the HEBM process and without formation of liquid Se (and Te), which could avoid the huge volume expansion. The other is the obvious decrease of sintering temperature and dwell time due to the effective shortened length of diffusion paths. The superconducting critical temperature Tc of 14.2 K in our sample is comparable with those in previous reports, and further optimization of chemical composition is on the way.

Nanostructured Mg 2Ni materials prepared by cold rolling and used as negative electrode for Ni-MH batteries

NASA Astrophysics Data System (ADS)

Pedneault, Sylvain; Huot, Jacques; Roué, Lionel

In the present work, cold rolling has been investigated as a new means of producing Mg-based metal hydrides for nickel-metal hydride (Ni-MH) batteries. Structure and electrochemical evolution of 2Mg-Ni cold-rolled samples were investigated as a function of the number of rolling passes as well as heat treatment. It was found that nanocrystalline Mg 2Ni alloy can be obtained by an appropriate three step process involving rolling, heat treatment and rolling again. It was shown that the number of primary and secondary rolling passes must be carefully optimized in order to favour the complete formation of Mg 2Ni alloy having a nanocrystalline structure (∼10 nm in crystallite size) without excessive sample oxidation. Actually, the best result was obtained by first rolling 90 times, followed by a heat treatment at 400 °C for 4 h and roll again 20 times. The resulting material displayed an initial discharge capacity of 205 mAh g -1, which is quite similar to that obtained with ball-milled Mg 2Ni alloy.

CHARACTERISTICS OF THERMOLUMINESCENCE LiF:Mg,Cu,Ag NANOPHOSPHOR.

PubMed

Yahyaabadi, A; Torkzadeh, F; Rezaei-Ochbelagh, D

2018-04-23

A nanophosphor of LiF:Mg,Cu,Ag was prepared by planetary ball milling for the first time in the laboratory. The size and shape of the nanophosphor were confirmed by XRD and SEM, which showed that it was cubic in shape and ~53 nm in size. The thermoluminescence (TL) characteristics of this nanophosphor were then investigated. It was found that the optimum annealing condition was 250°C for 10 min. The TL sensitivity of the prepared nanopowder was less than that of its micropowder counterpart and the TL glow curve structure exhibited several peaks. The LiF:Mg,Cu,Ag nanophosphor exhibited a linear response over a range of doses from 1 Gy to ~10 kGy. From this study, it appears that LiF:Mg,Cu,Ag nanophosphor is a good candidate for dosimetry because of its linearity over a range of doses, low tendency to fade, good repeatability and simple glow curve structure.

An example of how to handle amorphous fractions in API during early pharmaceutical development: SAR114137--a successful approach.

PubMed

Petzoldt, Christine; Bley, Oliver; Byard, Stephen J; Andert, Doris; Baumgartner, Bruno; Nagel, Norbert; Tappertzhofen, Christoph; Feth, Martin Philipp

2014-04-01

The so-called pharmaceutical solid chain, which encompasses drug substance micronisation to the final tablet production, at pilot plant scale is presented as a case study for a novel, highly potent, pharmaceutical compound: SAR114137. Various solid-state analytical methods, such as solid-state Nuclear Magnetic Resonance (ssNMR), Differential Scanning Calorimetry (DSC), Dynamic Water Vapour Sorption Gravimetry (DWVSG), hot-stage Raman spectroscopy and X-ray Powder Diffraction (XRPD) were applied and evaluated to characterise and quantify amorphous content during the course of the physical treatment of crystalline active pharmaceutical ingredient (API). DSC was successfully used to monitor the changes in amorphous content during micronisation of the API, as well as during stability studies. (19)F solid-state NMR was found to be the method of choice for the detection and quantification of low levels of amorphous API, even in the final drug product (DP), since compaction during tablet manufacture was identified as a further source for the formation of amorphous API. The application of different jet milling techniques was a critical factor with respect to amorphous content formation. In the present case, the change from spiral jet milling to loop jet milling led to a decrease in amorphous API content from 20-30 w/w% to nearly 0 w/w% respectively. The use of loop jet milling also improved the processability of the API. Stability investigations on both the milled API and the DP showed a marked tendency for recrystallisation of the amorphous API content on exposure to elevated levels of relative humidity. No significant impact of amorphous API on either the chemical stability or the dissolution rate of the API in drug formulation was observed. Therefore, the presence of amorphous content in the oral formulation was of no consequence for the clinical trial phases I and II. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of wet grinding on structural properties of ball clay

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purohit, A., E-mail: anuradha.purohit34@gmail.com; Chander, S.; Dhaka, M. S.

2015-05-15

In this paper, the effect of wet grinding on structural properties of ball clay is undertaken. The wet grinding treatment was performed employing ball and vibro mills for different time spells of 2, 4, 8 and 16 hours. The structural properties were carried out using X-ray diffraction (XRD). The structure of ground samples is found to be simple cubic. The crystallographic parameters are calculated and slight change in lattice constant, inter planner spacing and particle size is observed with grinding treatment. The results are in agreement with the available literature.

Composites Strengthened with Graphene Platelets and Formed in Semisolid State Based on α and α/β MgLiAl Alloys

NASA Astrophysics Data System (ADS)

Dutkiewicz, Jan; Rogal, Łukasz; Fima, Przemyslaw; Ozga, Piotr

2018-04-01

MgLiAl base composites strengthened with graphene platelets were prepared by semisolid processing of ball-milled alloy chips with 2% of graphene platelets. Composites strengthened with graphene platelets show higher hardness and yield stress than the cast alloys, i.e., 160 MPa as compared to 90 MPa for as-cast alloy MgLi9Al1.5. Mechanical properties for MgLiAl-based composites were similar or higher than for composites based on conventional AZ91 or WE43 alloys. The strengthening however was not only due to the presence of graphene, but also phases resulting from the reaction between carbon and lithium, i.e., Li2C2 carbide. Graphene platelets were located at globules boundaries resulting from semisolid processing for all investigated composites. Graphene platelets were in agglomerates forming continuous layers at grain boundaries in the composite based on the alloy MgLi4.5Al1.5. The shape of agglomerates was more complex and wavy in the composite based on MgLi9Al1.5 alloy most probably due to lithium-graphene reaction. Electron diffraction from the two-phase region α + β in MgLi9Al1.5 indicated that [001]α and [110]β directions are rotated about 4° from the ideal relationship [001] hex || [110] bcc phases. It showed higher lattice rotation than in earlier studies what is most probably caused by lattice slip and rotation during semisolid pressing causing substantial deformation particularly within the β phase. Raman spectroscopy studies confirmed the presence of graphene platelets within agglomerates and in addition the presence mainly of Li2C2 carbides in composites based on MgLi4.5Al1.5 and Mg9Li1.5Al alloys. From the character of Raman spectra refinement of graphene platelets was found in comparison with their initial size. The graphene areas without carbides contain graphene nanoplatelets with lateral dimension close to initial graphene sample. Electron diffraction allowed to confirm the presence of Li2C2 carbide at the surface of agglomerates found from

Composites Strengthened with Graphene Platelets and Formed in Semisolid State Based on α and α/β MgLiAl Alloys

NASA Astrophysics Data System (ADS)

Dutkiewicz, Jan; Rogal, Łukasz; Fima, Przemyslaw; Ozga, Piotr

2018-05-01

MgLiAl base composites strengthened with graphene platelets were prepared by semisolid processing of ball-milled alloy chips with 2% of graphene platelets. Composites strengthened with graphene platelets show higher hardness and yield stress than the cast alloys, i.e., 160 MPa as compared to 90 MPa for as-cast alloy MgLi9Al1.5. Mechanical properties for MgLiAl-based composites were similar or higher than for composites based on conventional AZ91 or WE43 alloys. The strengthening however was not only due to the presence of graphene, but also phases resulting from the reaction between carbon and lithium, i.e., Li2C2 carbide. Graphene platelets were located at globules boundaries resulting from semisolid processing for all investigated composites. Graphene platelets were in agglomerates forming continuous layers at grain boundaries in the composite based on the alloy MgLi4.5Al1.5. The shape of agglomerates was more complex and wavy in the composite based on MgLi9Al1.5 alloy most probably due to lithium-graphene reaction. Electron diffraction from the two-phase region α + β in MgLi9Al1.5 indicated that [001]α and [110]β directions are rotated about 4° from the ideal relationship [001] hex || [110] bcc phases. It showed higher lattice rotation than in earlier studies what is most probably caused by lattice slip and rotation during semisolid pressing causing substantial deformation particularly within the β phase. Raman spectroscopy studies confirmed the presence of graphene platelets within agglomerates and in addition the presence mainly of Li2C2 carbides in composites based on MgLi4.5Al1.5 and Mg9Li1.5Al alloys. From the character of Raman spectra refinement of graphene platelets was found in comparison with their initial size. The graphene areas without carbides contain graphene nanoplatelets with lateral dimension close to initial graphene sample. Electron diffraction allowed to confirm the presence of Li2C2 carbide at the surface of agglomerates found from

Synthesis and structural study of Ti-rich Mg-Ti hydrides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asano, Kohta; Kim, Hyunjeong; Sakaki, Kouji

2014-02-26

Mg xTi 1-x (x = 0.15, 0.25, 0.35) alloys were synthesized by means of ball milling. Under a hydrogen pressure of 8 MPa at 423 K these Mg–Ti alloys formed a hydride phase with a face centered cubic (FCC) structure. The hydride for x = 0.25 consisted of single Mg 0.25Ti 0.75H 1.62 FCC phase but TiH 2 and MgH 2 phases were also formed in the hydrides for x = 0.15 and 0.35, respectively. X-ray diffraction patterns and the atomic pair distribution function indicated that numbers of stacking faults were introduced. There was no sign of segregation between Mgmore » and Ti in Mg 0.25Ti 0.75H 1.62. Electronic structure of Mg 0.25Ti 0.75H 1.62 was different from those of MgH 2 and TiH 2, which was demonstrated by 1H nuclear magnetic resonance. This strongly suggested that stable Mg–Ti hydride phase was formed in the metal composition of Mg 0.25Ti 0.75 without disproportion into MgH 2 and TiH 2.« less

Mesoscale modeling of strain induced solid state amorphization in crystalline materials

NASA Astrophysics Data System (ADS)

Lei, Lei

Solid state amorphization, and in particular crystalline to amorphous transformation, can be observed in metallic alloys, semiconductors, intermetallics, minerals, and also molecular crystals when they undergo irradiation, hydrogen gas dissolution, thermal interdiffusion, mechanical alloying, or mechanical milling. Although the amorphization mechanisms may be different, the transformation occurs due to the high level of disorder introduced into the material. Milling induced solid state amorphization is proposed to be the result of accumulation of crystal defects, specifically dislocations, as the material is subjected to large deformations during the high energy process. Thus, understanding the deformation mechanisms of crystalline materials will be the first step in studying solid state amorphization in crystalline materials, which not only has scientific contributions, but also technical consequences. A phase field dislocation dynamics (PFDD) approach is employed in this work to simulate plastic deformation of molecular crystals. This PFDD model has the advantage of tracking all of the dislocations in a material simultaneously. The model takes into account the elastic interaction between dislocations, the lattice resistance to dislocation motion, and the elastic interaction of dislocations with an external stress field. The PFDD model is employed to describe the deformation of molecular crystals with pharmaceutical applications, namely, single crystal sucrose, acetaminophen, gamma-indomethacin, and aspirin. Stress-strain curves are produced that result in expected anisotropic material response due to the activation of different slip systems and yield stresses that agree well with those from experiments. The PFDD model is coupled to a phase transformation model to study the relation between plastic deformation and the solid state amorphization of crystals that undergo milling. This model predicts the amorphous volume fraction in excellent agreement with

Science of Ball Lightning (Fire Ball)

NASA Astrophysics Data System (ADS)

Ohtsuki, Yoshi-Hiko

1989-08-01

The Table of Contents for the full book PDF is as follows: * Organizing Committee * Preface * Ball Lightning -- The Continuing Challenge * Hungarian Ball Lightning Observations in 1987 * Nature of Ball Lightning in Japan * Phenomenological and Psychological Analysis of 150 Austrian Ball Lightning Reports * Physical Problems and Physical Properties of Ball Lightning * Statistical Analysis of the Ball Lightning Properties * A Fluid-Dynamical Model for Ball Lightning and Bead Lightning * The Lifetime of Hill's Vortex * Electrical and Radiative Properties of Ball Lightning * The Candle Flame as a Model of Ball Lightning * A Model for Ball Lightning * The High-Temperature Physico-Chemical Processes in the Lightning Storm Atmosphere (A Physico-Chemical Model of Ball Lightning) * New Approach to Ball Lightning * A Calculation of Electric Field of Ball Lightning * The Physical Explanation to the UFO over Xinjiang, Northern West China * Electric Reconnection, Critical Ionization Velocity, Ponderomotive Force, and Their Applications to Triggered and Ball Lightning * The PLASMAK™ Configuration and Ball Lightning * Experimental Research on Ball Lightning * Performance of High-Voltage Test Facility Designed for Investigation of Ball Lightning * List of Participants

Hydrogen storage properties of nanosized MgH2-0.1TiH2 prepared by ultrahigh-energy-high-pressure milling.

PubMed

Lu, Jun; Choi, Young Joon; Fang, Zhigang Zak; Sohn, Hong Yong; Rönnebro, Ewa

2009-11-04

Magnesium hydride (MgH(2)) is an attractive candidate for solid-state hydrogen storage applications. To improve the kinetics and thermodynamic properties of MgH(2) during dehydrogenation-rehydrogenation cycles, a nanostructured MgH(2)-0.1TiH(2) material system prepared by ultrahigh-energy-high-pressure mechanical milling was investigated. High-resolution transmission electron microscope (TEM) and scanning TEM analysis showed that the grain size of the milled MgH(2)-0.1TiH(2) powder is approximately 5-10 nm with uniform distributions of TiH(2) among MgH(2) particles. Pressure-composition-temperature (PCT) analysis demonstrated that both the nanosize and the addition of TiH(2) contributed to the significant improvement of the kinetics of dehydrogenation and hydrogenation compared to commercial MgH(2). More importantly, PCT cycle analysis demonstrated that the MgH(2)-0.1TiH(2) material system showed excellent cycle stability. The results also showed that the DeltaH value for the dehydrogenation of nanostructured MgH(2)-0.1TiH(2) is significantly lower than that of commercial MgH(2). However, the DeltaS value of the reaction was also lower, which results in minimum net effects of the nanosize and the addition of TiH(2) on the equilibrium pressure of dehydrogenation reaction of MgH(2).

Ultrathin IBAD MgO films for epitaxial growth on amorphous substrates and sub-50 nm membranes

DOE PAGES

Wang, Siming; Antonakos, C.; Bordel, C.; ...

2016-11-07

Here, a fabrication process has been developed for high energy ion beam assisted deposition (IBAD) biaxial texturing of ultrathin (~1 nm) MgO films, using a high ion-to-atom ratio and post-deposition annealing instead of a homoepitaxial MgO layer. These films serve as the seed layer for epitaxial growth of materials on amorphous substrates such as electron/X-ray transparent membranes or nanocalorimetry devices. Stress measurements and atomic force microscopy of the MgO films reveal decreased stress and surface roughness, while X-ray diffraction of epitaxial overlayers demonstrates the improved crystal quality of films grown epitaxially on IBAD MgO. The process simplifies the synthesis ofmore » IBAD MgO, fundamentally solves the “wrinkle” issue induced by the homoepitaxial layer on sub-50 nm membranes, and enables studies of epitaxial materials in electron/X-ray transmission and nanocalorimetry.« less

The influence of mineralogical, chemical and physical properties on grindability of commercial clinkers with high MgO level

DOE Office of Scientific and Technical Information (OSTI.GOV)

Souza, Vladia Cristina G. de; Koppe, Jair Carlos; Costa, Joao F.C.L.

2008-08-15

This research investigates various methods able to identify possible mineralogical, physical and chemical influences on the grindability of commercial clinkers with high MgO level. The aim of the study is to evaluate the hardness and elastic modulus of the clinker mineral phases and their fracture strength during the comminution processes, comparing samples from clinkers with low MgO level (0.5%) and clinkers with elevated MgO levels (> 5.0%). The study of the influence of mineralogical, chemical and physical properties was carried out using several analytical techniques, such as: optical microscopy, X-ray diffraction with Rietveld refinement (XRD) and X-ray fluorescence (XRF). Thesemore » techniques were useful in qualifying the different clinker samples. The drop weight test (DWT) and the Bond ball mill grindability test were performed to characterize the mechanical properties of clinkers. Nanoindentation tests were also carried out. Results from the Bond ball mill grindability test were found to be related to the hardness of the mineral phase and to mineralogical characteristics, such as type and amount of inclusions in silicates, belite and alite crystals shape, or microcracked alites. In contrast, the results obtained by the DWT were associated to the macro characteristics of clinkers, such as porosity, as well as to the hardness and mineralogical characteristics of belite crystals in clusters. Hardness instrumented tests helped to determine the Vickers hardness and elastic modulus from the mineral phases in commercial clinkers and produced different values for the pure phases compared to previous publications.« less

Nd2Fe14C-based magnet with better permanent magnetic properties prepared by a simple mechanochemical method

NASA Astrophysics Data System (ADS)

Geng, Hongmin; Ji, Yuan; Zhang, Jingjing; Gao, Yuchao; Yan, Yu; Wang, Wenquan; Su, Feng; Du, Xiaobo

2017-11-01

Nd2Fe14C-based magnet is prepared by a mechanochemical method, namely high-energy ball-milling Nd2Fe11Bx (x = 0-0.15) alloy in heptane (C7H16), followed by annealing to 850 °C in vacuum. Under the action of high-energy ball-milling, Nd2Fe11Bx react with heptane to form NdH2+δ, Fe-(CB), C, etc. H2 is released and Nd2Fe17, Nd2Fe17Cx (x = 0-3), Nd2Fe14C, Nd carbides and α-Fe are formed in the subsequent annealing. C amount depends on ball-milling time t. Long time ball milling or high C content suppresses the formation of 2:17 phase and favors the formation of 2:14:1 phase in the final products. Excessive ball-milling results in the quick increase of α-Fe. The maximum of magnetically hard Nd2Fe14C is obtained at t = 4 h. For Nd2Fe11 samples, there exists considerable quantity of Nd carbides and α-Fe phase appears earlier and increases rapidly with extending the ball-milling time t. The addition of B element shortens the ball-milling time of the formation of maximum Nd2Fe14C and prominently suppresses the formation of Nd carbide and α-Fe. The optimum magnetic properties, coercivity iHc of 1193.7 kA/m, remanence Mr of 580.9 kA/m, maximum magnetic energy product (BH)max of 91.7 kJ/m3 is approaching to its theoretic value of 99.2 kJ/m3 for isotropic Nd2Fe14C magnet, are obtained in Nd2Fe11B0.06 alloy ball milled for 3.5 h.

Pulsed current activated synthesis and rapid consolidation of a nanostructured Mg2Al4Si5O18 and its mechanical properties

NASA Astrophysics Data System (ADS)

Shon, In-Jin; Kang, Hyun-Su; Doh, Jung-Mann; Yoon, Jin-Kook

2015-03-01

Nanocrystalline materials have received much attention as advanced engineering materials, with improved mechanical properties. Attention has been directed to the application of nanomaterials, as they possess excellent mechanical properties (high strength, high hardness, excellent ductility and toughness). A singlestep synthesis and consolidation of nanostructured Mg2Al4Si5O18 was achieved by pulsed current heating, using the stoichiometric mixture of MgO, Al2O3 and SiO2 powders. Before sintering, the powder mixture was high-energy ball milled for 10 h. From the milled powder mixture, a highly dense nanostructured Mg2Al4Si5O18 compound could be obtained within one minute, under the simultaneous application of 80 MPa pressure, and a pulsed current. The advantage of this process is that it allows an instant densification to the near theoretical density, while sustaining the nanosized microstructure of raw powders. The sintering behavior, microstructure and mechanical properties of Mg2Al4Si5O18 were evaluated. The fracture toughness of a nanostructured Mg2Al4Si5O18 compound was higher than that of sub-micron Mg2Al4Si5O18 compound.

A comparison of field-dependent rheological properties between spherical and plate-like carbonyl iron particles-based magneto-rheological fluids

NASA Astrophysics Data System (ADS)

Tan Shilan, Salihah; Amri Mazlan, Saiful; Ido, Yasushi; Hajalilou, Abdollah; Jeyadevan, Balachandran; Choi, Seung-Bok; Azhani Yunus, Nurul

2016-09-01

This work proposes different sizes of the plate-like particles from conventional spherical carbonyl iron (CI) particles by adjusting milling time in the ball mill process. The ball mill process to make the plate-like particles is called a solid-state powder processing technique which involves repeated welding, fracturing and re-welding of powder particles in a high-energy ball mill. The effect of ball milling process on the magnetic behavior of CI particles is firstly investigated by vibrating sample magnetometer. It is found form this investigation that the plate-like particles have higher saturation magnetization (about 8%) than that of the spherical particles. Subsequently, for the investigation on the sedimentation behavior the cylindrical measurement technique is used. It is observed from this measurement that the plate-like particles show slower sedimentation rate compared to the spherical particles indicating higher stability of the MR fluid. The field-dependent rheological properties of MR fluids based on the plate-like particles are then investigated with respect to the milling time which is directly connected to the size of the plate-like particles. In addition, the field-dependent rheological properties such as the yield stress are evaluated and compared between the plate-like particles based MR fluids and the spherical particles based MR fluid. It is found that the yield shear stress of the plate-like particles based MR fluid is increased up to 270% compared to the spherical particles based MR fluid.

An innovative technique to synthesize C-doped MgB2 by using chitosan as the carbon source

NASA Astrophysics Data System (ADS)

Bovone, G.; Vignolo, M.; Bernini, C.; Kawale, S.; Siri, A. S.

2014-02-01

Here, we report a new technique to synthesize carbon-doped MgB2 powder. Chitosan was innovatively used as the carbon source during the synthesis of boron from boron oxide. This allowed the introduction of local defects, which later on served as pinning centers in MgB2, in the boron lattice itself, avoiding the traditional and time consuming ways of ex situ MgB2 doping (e.g. ball milling). Two volume percentages of C-doping have been tried and its effect on the superconducting properties, evaluated by magnetic and transport measurements, are discussed here. Morphological analysis by scanning electron microscopy revealed nano-metric grains’ distribution in the boron and MgB2 powder. Mono-filamentary MgB2 wires have been fabricated by an ex situ powder-in-tube technique by using the thus prepared carbon-doped MgB2 and pure MgB2 powders. Transport property measurements on these wires were made and compared with MgB2 wire produced using commercial boron.

Nanocrystalline Fe/Zr alloys: preparation by using mechanical alloying and mechanical milling processes

NASA Astrophysics Data System (ADS)

Rodríguez, V. A. Peña; Medina, J. Medina; Marcatoma, J. Quispe; Ayala, Ch. Rojas; Landauro, C. V.; Baggio-Saitovitch, E. M.; Passamani, E. C.

2011-11-01

Nanocrystalline Fe/Zr alloys have been prepared after milling for 9 h the mixture of elemental Fe and Zr powders or the arc-melting produced Fe2Zr alloy by using mechanical alloying and mechanical milling techniques, respectively. X-ray and Mössbauer results of the Fe and Zr powders, mechanically alloyed, suggest that amorphous Fe2Zr phase and \\upalpha-Fe(Zr) nanograins have been produced with relative concentrations of 91% and 9%, respectively. Conversely, the results of the mechanically milled Fe2Zr alloy indicate that nanograins of the Fe2Zr alloy have been formed, surrounded by a magnetic inter-granular phase that are simultaneously dispersed in a paramagnetic amorphous phase.

The Structure and Mechanical Properties of High-Strength Bulk Ultrafine-Grained Cobalt Prepared Using High-Energy Ball Milling in Combination with Spark Plasma Sintering

PubMed Central

Marek, Ivo; Vojtěch, Dalibor; Michalcová, Alena; Kubatík, Tomáš František

2016-01-01

In this study, bulk ultrafine-grained and micro-crystalline cobalt was prepared using a combination of high-energy ball milling and subsequent spark plasma sintering. The average grain sizes of the ultrafine-grained and micro-crystalline materials were 200 nm and 1 μm, respectively. Mechanical properties such as the compressive yield strength, the ultimate compressive strength, the maximum compressive deformation and the Vickers hardness were studied and compared with those of a coarse-grained as-cast cobalt reference sample. The bulk ultrafine-grained sample showed an ultra-high compressive yield strength that was greater than 1 GPa, which is discussed with respect to the preparation technique and a structural investigation. PMID:28773514

Demonstration of a silicon nitride attrition mill for production of fine pure Si and Si3N4 powders

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.; Orth, N. W.

1984-01-01

To avoid metallic impurities normally introduced by milling ceramic powders in conventional steel hardware, an attrition mill (high-energy stirred ball mill) was constructed with the wearing parts (mill body, stirring arms, and media) made from silicon nitride. Commercial silicon and Si3N4 powders were milled to fine uniform particles with only minimal contamination - primarily from wear of the sintered Si3N4 media.

Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data

PubMed Central

García Nieto, Paulino José; García-Gonzalo, Esperanza; Ordóñez Galán, Celestino; Bernardo Sánchez, Antonio

2016-01-01

Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC) in combination with multivariate adaptive regression splines (MARS) technique. This optimization mechanism involved the parameter setting in the MARS training procedure, which significantly influences the regression accuracy. Therefore, an ABC–MARS-based model was successfully used here to predict the milling tool flank wear (output variable) as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc. Regression with optimal hyperparameters was performed and a determination coefficient of 0.94 was obtained. The ABC–MARS-based model's goodness of fit to experimental data confirmed the good performance of this model. This new model also allowed us to ascertain the most influential parameters on the milling tool flank wear with a view to proposing milling machine's improvements. Finally, conclusions of this study are exposed. PMID:28787882

Hybrid ABC Optimized MARS-Based Modeling of the Milling Tool Wear from Milling Run Experimental Data.

PubMed

García Nieto, Paulino José; García-Gonzalo, Esperanza; Ordóñez Galán, Celestino; Bernardo Sánchez, Antonio

2016-01-28

Milling cutters are important cutting tools used in milling machines to perform milling operations, which are prone to wear and subsequent failure. In this paper, a practical new hybrid model to predict the milling tool wear in a regular cut, as well as entry cut and exit cut, of a milling tool is proposed. The model was based on the optimization tool termed artificial bee colony (ABC) in combination with multivariate adaptive regression splines (MARS) technique. This optimization mechanism involved the parameter setting in the MARS training procedure, which significantly influences the regression accuracy. Therefore, an ABC-MARS-based model was successfully used here to predict the milling tool flank wear (output variable) as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc . Regression with optimal hyperparameters was performed and a determination coefficient of 0.94 was obtained. The ABC-MARS-based model's goodness of fit to experimental data confirmed the good performance of this model. This new model also allowed us to ascertain the most influential parameters on the milling tool flank wear with a view to proposing milling machine's improvements. Finally, conclusions of this study are exposed.

Fabrication of Metallic Glass Powder for Brazing Paste for High-Temperature Thermoelectric Modules

NASA Astrophysics Data System (ADS)

Seo, Seung-Ho; Kim, Suk Jun; Lee, Soonil; Seo, Won-Seon; Kim, Il-Ho; Choi, Soon-Mok

2018-06-01

Metallic glass (MG) offers the advantage of outstanding oxidation resistance, since it has disordered atomic-scale structure without grain boundaries. We fabricated Al-based MG ribbons (Al84.5Y10Ni5.5) by a melt spinning process. We evaluated the adhesion strength of interfaces between the Al-based MG and a Ni-coated Cu electrode formed under various conditions at high temperature. In addition, we attempted to optimize the process conditions for pulverizing MG ribbons to < 100 micrometers by combining high-energy ball milling and planetary milling. We confirmed that the electrical resistivity of the Al-based MG ribbon was substantially reduced after annealing at high temperature (over 300°C) due to crystallization.

Development of an Mg-Based Alloy with a Hydrogen-Storage Capacity over 6 wt% by Adding Graphene

NASA Astrophysics Data System (ADS)

Choi, Eunho; Kwak, Young Jun; Song, Myoung Youp

2018-06-01

Graphene (multilayer graphene) was chosen as an additive to improve the hydrogen uptake and release properties of magnesium (Mg). Five weight percent of graphene was added to pre-milled Mg by milling in hydrogen (reaction-involving milling). The hydrogen uptake and release properties of the graphene-added Mg were investigated. The activation of Mg-5graphene, which was prepared by adding 5 wt% graphene to Mg pre-milled for 24 h, was completed after the second cycle (cycle number, CN = 2). Mg-5graphene had a high effective hydrogen-storage capacity (the quantity of hydrogen absorbed for 60 min) of 6.21 wt% at CN = 3 at 593 K in 12 bar H2. At CN = 1, Mg-5graphene released 0.46 wt% hydrogen for 10 min and 4.99 wt% hydrogen for 60 min. Milling in hydrogen is believed to create defects (leading to facilitation of nucleation), produce cracks and clean surfaces (leading to increase in reactivity), and decrease particle size (leading to diminution of diffusion distances or increasing the flux of diffusing hydrogen atoms). The added graphene is believed to have helped the sample have higher hydrogen uptake and release rates, weakly but partly, by dispersing heat rapidly.

Effect of milling methods on performance of Ni-Y 2O 3-stabilized ZrO 2 anode for solid oxide fuel cell

NASA Astrophysics Data System (ADS)

Cho, Hyoup Je; Choi, Gyeong Man

A Ni-YSZ (Y 2O 3-stabilized ZrO 2) composite is commonly used as a solid oxide fuel cell anode. The composite powders are usually synthesized by mixing NiO and YSZ powders. The particle size and distribution of the two phases generally determine the performance of the anode. Two different milling methods are used to prepare the composite anode powders, namely, high-energy milling and ball-milling that reduce the particle size. The particle size and the Ni distribution of the two composite powders are examined. The effects of milling on the performance are evaluated by using both an electrolyte-supported, symmetric Ni-YSZ/YSZ/Ni-YSZ cell and an anode-supported, asymmetric cell. The performance is examined at 800 °C by impedance analysis and current-voltage measurements. Pellets made by using high-energy milled NiO-YSZ powders have much smaller particle sizes and a more uniform distribution of Ni particles than pellets made from ball-milled powder, and thus the polarization resistance of the electrode is also smaller. The maximum power density of the anode-supported cell prepared by using the high-energy milled powder is ∼850 mW cm -2 at 800 °C compared with ∼500 mW cm -2 for the cell with ball-milled powder. Thus, high-energy milling is found to be more effective in reducing particle size and obtaining a uniform distribution of Ni particles.

Individual ball possession in soccer

PubMed Central

Hoernig, Martin

2017-01-01

This paper describes models for detecting individual and team ball possession in soccer based on position data. The types of ball possession are classified as Individual Ball Possession (IBC), Individual Ball Action (IBA), Individual Ball Control (IBC), Team Ball Possession (TBP), Team Ball Control (TBC) und Team Playmaking (TPM) according to different starting points and endpoints and the type of ball control involved. The machine learning approach used is able to determine how long the ball spends in the sphere of influence of a player based on the distance between the players and the ball together with their direction of motion, speed and the acceleration of the ball. The degree of ball control exhibited during this phase is classified based on the spatio-temporal configuration of the player controlling the ball, the ball itself and opposing players using a Bayesian network. The evaluation and application of this approach uses data from 60 matches in the German Bundesliga season of 2013/14, including 69,667 IBA intervals. The identification rate was F = .88 for IBA and F = .83 for IBP, and the classification rate for IBC was κ = .67. Match analysis showed the following mean values per match: TBP 56:04 ± 5:12 min, TPM 50:01 ± 7:05 min and TBC 17:49 ± 8:13 min. There were 836 ± 424 IBC intervals per match and their number was significantly reduced by -5.1% from the 1st to 2nd half. The analysis of ball possession at the player level indicates shortest accumulated IBC times for the central forwards (0:49 ± 0:43 min) and the longest for goalkeepers (1:38 ± 0:58 min), central defenders (1:38 ± 1:09 min) and central midfielders (1:27 ± 1:08 min). The results could improve performance analysis in soccer, help to detect match events automatically, and allow discernment of higher value tactical structures, which is based on individual ball possession. PMID:28692649

Formation of an amorphous phase and its crystallization in the immiscible Nb-Zr system by mechanical alloying

NASA Astrophysics Data System (ADS)

Al-Aqeeli, N.; Suryanarayana, C.; Hussein, M. A.

2013-10-01

Mechanical alloying of binary Nb-Zr powder mixtures was carried out to evaluate the formation of metastable phases in this immiscible system. The milled powders were characterized for their constitution and structure by X-ray diffraction and transmission electron microscopy methods. It was shown that an amorphous phase had formed on milling the binary powder mixture for about 10 h and that it had crystallized on subsequent milling up to 50-70 h, referred to as mechanical crystallization. Thermodynamic and structural arguments have been presented to explain the formation of the amorphous phase and its subsequent crystallization.

Low-temperature MIR to submillimeter mass absorption coefficient of interstellar dust analogues. II. Mg and Fe-rich amorphous silicates

NASA Astrophysics Data System (ADS)

Demyk, K.; Meny, C.; Leroux, H.; Depecker, C.; Brubach, J.-B.; Roy, P.; Nayral, C.; Ojo, W.-S.; Delpech, F.

2017-10-01

Context. To model the cold dust emission observed in the diffuse interstellar medium, in dense molecular clouds or in cold clumps that could eventually form new stars, it is mandatory to know the physical and spectroscopic properties of this dust and to understand its emission. Aims: This work is a continuation of previous studies aiming at providing astronomers with spectroscopic data of realistic cosmic dust analogues for the interpretation of observations. The aim of the present work is to extend the range of studied analogues to iron-rich silicate dust analogues. Methods: Ferromagnesium amorphous silicate dust analogues were produced by a sol-gel method with a mean composition close to Mg1-xFexSiO3 with x = 0.1, 0.2, 0.3, 0.4. Part of each sample was annealed at 500 °C for two hours in a reducing atmosphere to modify the oxidation state of iron. We have measured the mass absorption coefficient (MAC) of these eight ferromagnesium amorphous silicate dust analogues in the spectral domain 30-1000 μm for grain temperature in the range 10-300 K and at room temperature in the 5-40 μm range. Results: The MAC of ferromagnesium samples behaves in the same way as the MAC of pure Mg-rich amorphous silicate samples. In the 30-300 K range, the MAC increases with increasing grain temperature whereas in the range 10-30 K, we do not see any change of the MAC. The MAC cannot be described by a single power law in λ- β. The MAC of the samples does not show any clear trend with the iron content. However the annealing process has, on average, an effect on the MAC that we explain by the evolution of the structure of the samples induced by the processing. The MAC of all the samples is much higher than the MAC calculated by dust models. Conclusions: The complex behavior of the MAC of amorphous silicates with wavelength and temperature is observed whatever the exact silicate composition (Mg vs. Fe amount). It is a universal characteristic of amorphous materials, and therefore of

Effect of milling on particle shape and surface energy heterogeneity of needle-shaped crystals.

PubMed

Ho, Raimundo; Naderi, Majid; Heng, Jerry Y Y; Williams, Daryl R; Thielmann, Frank; Bouza, Peter; Keith, Adam R; Thiele, Greg; Burnett, Daniel J

2012-10-01

Milling and micronization of particles are routinely employed in the pharmaceutical industry to obtain small particles with desired particle size characteristics. The aim of this study is to demonstrate that particle shape is an important factor affecting the fracture mechanism in milling. Needle-shaped crystals of the β polymorph of D-mannitol were prepared from recrystallization in water. A portion of the recrystallized materials was ball-milled. Unmilled and milled sieved fractions of recrystallized D-mannitol were analyzed by dynamic image analysis (DIA) and inverse gas chromatography (IGC) at finite concentration to explain the breakage/fracture behavior. In the process of ball-milling, D-mannitol preferentially fractured along their shortest axis, exposing (011) plane with increased hydrophilicity and increased bounding rectangular aspect ratio. This is in contrary to attachment energy modeling which predicts a fracture mechanism across the (010) plane with increased hydrophobicity, and small change in particle shape. Crystal size, and more importantly, crystal shape and facet-specific mechanical properties, can dictate the fracture/cleavage behavior of organic crystalline materials. Thorough understanding of the crystal slip systems, combining attachment energy prediction with particle shape and surface characterization using DIA and IGC, are important in understanding fracture behavior of organic crystalline solids in milling and micronization.

Production and Characterization of Bulk MgB2 Material made by the Combination of Crystalline and Carbon Coated Amorphous Boron Powders

NASA Astrophysics Data System (ADS)

Hiroki, K.; Muralidhar, M.; Koblischka, M. R.; Murakami, M.

2017-07-01

The object of this investigation is to reduce the cost of bulk production and in the same time to increase the critical current performance of bulk MgB2 material. High-purity commercial powders of Mg metal (99.9% purity) and two types of crystalline (99% purity) and 16.5 wt% carbon-coated, nanometer-sized amorphous boron powders (98.5% purity) were mixed in a nominal composition of MgB2 to reduce the boron cost and to see the effect on the superconducting and magnetic properties. Several samples were produced mixing the crystalline boron and carbon-coated, nanometer-sized amorphous boron powders in varying ratios (50:50, 60:40, 70:30, 80:20, 90:10) and synthesized using a single-step process using the solid state reaction around 800 °C for 3 h in pure argon atmosphere. The magnetization measurements exhibited a sharp superconducting transition temperature with T c, onset around 38.6 K to 37.2 K for the bulk samples prepared utilizing the mixture of crystalline boron and 16.5% carbon-coated amorphous boron. The critical current density at higher magnetic field was improved with addition of carbon-coated boron to crystalline boron in a ratio of 80:20. The highest self-field Jc around 215,000 A/cm2 and 37,000 A/cm2 were recorded at 20 K, self-field and 2 T for the sample with a ratio of 80:10. The present results clearly demonstrate that the bulk MgB2 performance can be improved by adding carbon-coated nano boron to crystalline boron, which will be attractive to reduce the cost of bulk MgB2 material for several industrial applications.

Facile Fabrication of 100% Bio-Based and Degradable Ternary Cellulose/PHBV/PLA Composites

PubMed Central

Wang, Jinwu

2018-01-01

Modifying bio-based degradable polymers such as polylactide (PLA) and poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) with non-degradable agents will compromise the 100% degradability of their resultant composites. This work developed a facile and solvent-free route in order to fabricate 100% bio-based and degradable ternary cellulose/PHBV/PLA composite materials. The effects of ball milling on the physicochemical properties of pulp cellulose fibers, and the ball-milled cellulose particles on the morphology and mechanical properties of PHBV/PLA blends, were investigated experimentally and statistically. The results showed that more ball-milling time resulted in a smaller particle size and lower crystallinity by way of mechanical disintegration. Filling PHBV/PLA blends with the ball-milled celluloses dramatically increased the stiffness at all of the levels of particle size and filling content, and improved their elongation at the break and fracture work at certain levels of particle size and filling content. It was also found that the high filling content of the ball-milled cellulose particles was detrimental to the mechanical properties for the resultant composite materials. The ternary cellulose/PHBV/PLA composite materials have some potential applications, such as in packaging materials and automobile inner decoration parts. Furthermore, filling content contributes more to the variations of their mechanical properties than particle size does. Statistical analysis combined with experimental tests provide a new pathway to quantitatively evaluate the effects of multiple variables on a specific property, and figure out the dominant one for the resultant composite materials. PMID:29495315

Energy release properties of amorphous boron and boron-based propellant primary combustion products

NASA Astrophysics Data System (ADS)

Liang, Daolun; Liu, Jianzhong; Xiao, Jinwu; Xi, Jianfei; Wang, Yang; Zhang, Yanwei; Zhou, Junhu

2015-07-01

The microstructure of amorphous boron and the primary combustion products of boron-based fuel-rich propellant (hereafter referred to as primary combustion products) was analyzed by scanning electron microscope. Composition analysis of the primary combustion products was carried out by X-ray diffraction and X-ray photoelectron spectroscopy. The energy release properties of amorphous boron and the primary combustion products were comparatively studied by laser ignition experimental system and thermogravimetry-differential scanning calorimetry. The primary combustion products contain B, C, Mg, Al, B4C, B13C2, BN, B2O3, NH4Cl, H2O, and so on. The energy release properties of primary combustion products are different from amorphous boron, significantly. The full-time spectral intensity of primary combustion products at a wavelength of 580 nm is ~2% lower than that of amorphous boron. The maximum spectral intensity of the former at full wave is ~5% higher than that of the latter. The ignition delay time of primary combustion products is ~150 ms shorter than that of amorphous boron, and the self-sustaining combustion time of the former is ~200 ms longer than that of the latter. The thermal oxidation process of amorphous boron involves water evaporation (weight loss) and boron oxidation (weight gain). The thermal oxidation process of primary combustion products involves two additional steps: NH4Cl decomposition (weight loss) and carbon oxidation (weight loss). CL-20 shows better combustion-supporting effect than KClO4 in both the laser ignition experiments and the thermal oxidation experiments.

Molecular implications of drug-polymer solubility in understanding the destabilization of solid dispersions by milling.

PubMed

Yang, Ziyi; Nollenberger, Kathrin; Albers, Jessica; Qi, Sheng

2014-07-07

The solubility of drugs in polymer matrixes has been recognized as one of the key factors governing the physical stability of solid dispersions. This study has explored the implications of drug solubility on the destabilization that occurs on milling, which is often used as an additional process for hot melt extruded (HME) solid dispersions. The theoretical drug solubility in the polymer was first predicted using various theoretical and experimental approaches. The destabilization effects of high-energy mechanical milling on the solid dispersions with drug loadings below and above the predicted solubility were then investigated using a range of thermal, microscopic, and spectroscopic techniques. Four model drug-polymer combinations were studied. The HME formulations with drug loading below the predicted solid solubility (undersaturated and true molecular dispersion) showed good stability against milling. In contrast, milling destabilized supersaturated HME dispersions via increasing molecular mobility and creating phase-separated, amorphous, drug-rich domains. However, these additional amorphous drug-rich domains created by milling show good stability under ambient conditions, though crystallization can be accelerated by additional heating. These results highlighted that the processing method used to prepare the solid dispersions may play a role in facilitating the stabilization of amorphous drug in supersaturated solid dispersions. The degree of supersaturation of the drug in the polymer showed significant impact on the destabilization behavior of milling on solid dispersions. An improved understanding of the destabilization behavior of solid dispersions upon milling can provide new insights into the processing related apparent solubility of drugs in polymers.

High hydrogen desorption properties of Mg-based nanocomposite at moderate temperatures: The effects of multiple catalysts in situ formed by adding nickel sulfides/graphene

NASA Astrophysics Data System (ADS)

Xie, Xiubo; Chen, Ming; Liu, Peng; Shang, Jiaxiang; Liu, Tong

2017-12-01

Nickel sulfides decorated reduced graphene oxide (rGO) has been produced by co-reducing Ni2+ and graphene oxide (GO), and is subsequently ball milled with Mg nanoparticles (NPs) produced by hydrogen plasma metal reaction (HPMR). The nickel sulfides of about 800 nm completely in situ change to MgS, Mg2Ni and Ni multiple catalysts after first hydrogenation/dehydrogenation process at 673 K. The Mg-5wt%NiS/rGO nanocomposite shows the highest hydrogen desorption kinetics and capacity properties, and the catalytic effect order of the additives is NiS/rGO, NiS and rGO. At 573 K, the Mg-NiS/rGO nanocomposite can quickly desorb 3.7 wt% H2 in 10 min and 4.5 wt% H2 in 60 min. The apparent hydrogen absorption and desorption activation energies of the Mg-5wt%NiS/rGO nanocomposite are decreased to 44.47 and 63.02 kJ mol-1, smaller than those of the Mg-5wt%rGO and Mg-5wt%NiS samples. The best hydrogen desorption properties of the Mg-5wt%NiS/rGO nanocomposite can be explained by the synergistic catalytic effects of the highly dispersed MgS, Mg2Ni and Ni catalysts on the rGO sheets, and the more nucleation sites between the catalysts, rGO sheets and Mg matrix.

Sport-Based Youth and Community Development: Beyond the Ball in Chicago

ERIC Educational Resources Information Center

Jacobs, Jennifer M.; Castañeda, Amy; Castañeda, Rob

2016-01-01

Rob and Amy Castañeda, the co-founders of a sports/play-based youth and community development organization called Beyond the Ball (www.beyondtheball.org), cite the collaborative and dynamic nature of the TPSR Alliance as an important influence for their work. Beyond the Ball serves individuals between kindergarten and post-college, in the North…

Optimization of the buffer surface of CoFeB/MgO/CoFeB-based magnetic tunnel junctions by ion beam milling

NASA Astrophysics Data System (ADS)

Martins, L.; Ventura, J.; Ferreira, R.; Freitas, P. P.

2017-12-01

Due to their high tunnel magnetoresistance (TMR) ratios at room temperature, magnetic tunnel junctions (MTJs) with a crystalline MgO insulating barrier and CoFeB ferromagnetic (FM) layers are the best candidates for novel magnetic memory applications. To overcome impedance matching problems in electronic circuits, the MgO barrier must have an ultra-low thickness (∼1 nm). Therefore, it is mandatory to optimize the MTJ fabrication process, in order to prevent relevant defects in the MgO barrier that could affect the magnetic and electrical MTJ properties. Here, a smoothing process aiming to decrease the roughness of the buffer surface before the deposition of the full MTJ stack is proposed. An ion beam milling process was used to etch the surface of an MTJ buffer structure with a Ru top layer. The morphologic results prove an effective decrease of the Ru surface roughness with the etching time. The electrical and magnetic results obtained for MTJs with smoothed buffer structures show a direct influence of the buffer roughness and coupling field on the improvement of the TMR ratio.

Cryo-Milling and the Hydrogen Storage Properties of NaAlH4

NASA Astrophysics Data System (ADS)

Feller, Kevin; Dobbins, Tabbetha

2013-03-01

High energy ball milling of metal hydrides is a common way to both introduce catalysts (e.g. TiCl3) and to simultaneously increase the surface area. Both catalysis and increased surface area improve hydrogen storage capacity of the material. Nanostructuring of hydrides by depositing them into mesoporous templates (such as anodized alumina, MOFs, and SBA-15) has become a common way to increase surface area. However, the mesoporous template does not add hydrogen storage capacity--and thus, tends to decreased overall storage weight percent for the nanostructured hydride material. As with most materials, hydrides become brittle at low temperatures and will tend to fracture more readily. We will process Sodium Aluminum Hydride (NaAlH4) using cryogenic high energy ball milling using an in-house modified chamber SPEX Certiprep M8000 mixer/mill in order to gain a nanostructured hydride without mesoporous template material. Details of the modified mixer mill design will be presented. Ultimately, our planned future work is to study the resultant material using x-ray diffraction (Scherrer method for crystallite size), absorption/desorption temperature programmed desorption (TPD), and ultrasmall-angle x-ray scattering (USAXS) microstructural quantification to understand the role of cryomilling on enhancing the material's ability to store (and release) hydrogen.

Atomic-scale compositional mapping reveals Mg-rich amorphous calcium phosphate in human dental enamel.

PubMed

La Fontaine, Alexandre; Zavgorodniy, Alexander; Liu, Howgwei; Zheng, Rongkun; Swain, Michael; Cairney, Julie

2016-09-01

Human dental enamel, the hardest tissue in the body, plays a vital role in protecting teeth from wear as a result of daily grinding and chewing as well as from chemical attack. It is well established that the mechanical strength and fatigue resistance of dental enamel are derived from its hierarchical structure, which consists of periodically arranged bundles of hydroxyapatite (HAP) nanowires. However, we do not yet have a full understanding of the in vivo HAP crystallization process that leads to this structure. Mg(2+) ions, which are present in many biological systems, regulate HAP crystallization by stabilizing its precursor, amorphous calcium phosphate (ACP), but their atomic-scale distribution within HAP is unknown. We use atom probe tomography to provide the first direct observations of an intergranular Mg-rich ACP phase between the HAP nanowires in mature human dental enamel. We also observe Mg-rich elongated precipitates and pockets of organic material among the HAP nanowires. These observations support the postclassical theory of amelogenesis (that is, enamel formation) and suggest that decay occurs via dissolution of the intergranular phase. This information is also useful for the development of more accurate models to describe the mechanical behavior of teeth.

Improved electrochemical properties of amorphous Mg 65Ni 27La 8 electrodes: Surface modification using graphite

NASA Astrophysics Data System (ADS)

Wu, D. C.; Li, Lu; Liang, G. Y.; Guo, Y. L.; Wu, H. B.

Amorphous Mg 65Ni 27La 8 alloy is prepared by melt-spinning. The alloy surface is modified using different contents of graphite to improve the performances of the Mg 65Ni 27La 8 electrodes. In detail, the electrochemical properties of (Mg 65Ni 27La 8) + xC (x = 0-0.4) electrodes are studied systematically, where x is the mass ratio of graphite to alloy. Experimental results reveal that the discharge capacity, cycle life, discharge potential characteristics and electrochemical kinetics of the electrodes are all improved. The surface modification enhances the electrocatalytic activity of the alloy, reduces the contact resistance of the electrodes and obstructs the formation of Mg(OH) 2 on the alloy surface. An optimal content of graphite has been obtained. The (Mg 65Ni 27La 8) + 0.25 C electrode has the largest discharge capacity of 827 mA h g -1, which is 1.47 times as large as that of the electrode without graphite, and the best electrochemical kinetics. Further increasing of graphite content will lead to the increase of contact resistance and activation energy for charge-transfer reaction of the electrode, resulting in the degradation of electrode performance.

Investigation of the capacity of low glass transition temperature excipients to minimize amorphization of sulfadimidine on comilling.

PubMed

Curtin, Vincent; Amharar, Youness; Hu, Yun; Erxleben, Andrea; McArdle, Patrick; Caron, Vincent; Tajber, Lidia; Corrigan, Owen I; Healy, Anne Marie

2013-01-07

The coprocessing of active pharmaceutical ingredient (API) with an excipient which has a high glass transition temperature (T(g)) is a recognized strategy to stabilize the amorphous form of a drug. This work investigates whether coprocessing a model API, sulfadimidine (SDM) with a series of low T(g) excipients, prevents or reduces amorphization of the crystalline drug. It was hypothesized that these excipients could exert a T(g) lowering effect, resulting in composite T(g) values lower than that of the API alone and promote crystallization of the drug. Milled SDM and comilled SDM with glutaric acid (GA), adipic acid (AA), succinic acid (SA), and malic acid (MA) were characterized with respect to their thermal, X-ray diffraction, spectroscopic, and vapor sorption properties. SDM was predominantly amorphous when milled alone, with an amorphous content of 82%. No amorphous content was detected by dynamic vapor sorption (DVS) on comilling SDM with 50% w/w GA, and amorphous content of the API was reduced by almost 30%, relative to the API milled alone, on comilling with 50% w/w AA. In contrast, amorphization of SDM was promoted on comilling with 50% w/w SA and MA, as indicated by near-infrared (NIR) spectroscopy. Results indicated that the API was completely amorphized in the SDM:MA comilled composite. The saturated solubility of GA and AA in the amorphous API was estimated by thermal methods. It was observed that the T(g) of the comelt quenched composites reached a minimum and leveled out at this solubility concentration. Maximum crystallinity of API on comilling was reached at excipient concentrations comparable to the saturated concentration solubility of excipient in the API. Moreover, the closer the Hildebrand solubility parameter of the excipient to the API, the greater the inhibition of API amorphization on comilling. The results reported here indicate that an excipient with a low T(g) coupled with high solubility in the API can prevent or reduce the generation

Process parameter dependent growth phenomena of naproxen nanosuspension manufactured by wet media milling.

PubMed

Bitterlich, A; Laabs, C; Krautstrunk, I; Dengler, M; Juhnke, M; Grandeury, A; Bunjes, H; Kwade, A

2015-05-01

The production of nanosuspensions has proved to be an effective method for overcoming bioavailability challenges of poorly water soluble drugs. Wet milling in stirred media mills and planetary ball mills has become an established top-down-method for producing such drug nanosuspensions. The quality of the resulting nanosuspension is determined by the stability against agglomeration on the one hand, and the process parameters of the mill on the other hand. In order to understand the occurring dependencies, a detailed screening study, not only on adequate stabilizers, but also on their optimum concentration was carried out for the active pharmaceutical ingredient (API) naproxen in a planetary ball mill. The type and concentration of the stabilizer had a pronounced influence on the minimum particle size obtained. With the best formulation the influence of the relevant process parameters on product quality was investigated to determine the grinding limit of naproxen. Besides the well known phenomenon of particle agglomeration, actual naproxen crystal growth and morphology alterations occurred during the process which has not been observed before. It was shown that, by adjusting the process parameters, those effects could be reduced or eliminated. Thus, besides real grinding and agglomeration a process parameter dependent ripening of the naproxen particles was identified to be a concurrent effect during the naproxen fine grinding process. Copyright © 2015 Elsevier B.V. All rights reserved.

Ball Screw Actuator Including a Compliant Ball Screw Stop

NASA Technical Reports Server (NTRS)

Wingett, Paul T. (Inventor); Hanlon, Casey (Inventor)

2015-01-01

An actuator includes a ball nut, a ball screw, and a ball screw stop. The ball nut is adapted to receive an input torque and in response rotates and supplies a drive force. The ball screw extends through the ball nut and has a first end and a second end. The ball screw receives the drive force from the ball nut and in response selectively translates between a retract position and a extend position. The ball screw stop is mounted on the ball screw proximate the first end to translate therewith. The ball screw stop engages the ball nut when the ball screw is in the extend position, translates, with compliance, a predetermined distance toward the first end upon engaging the ball nut, and prevents further rotation of the ball screw upon translating the predetermined distance.

Ball Screw Actuator Including a Compliant Ball Screw Stop

NASA Technical Reports Server (NTRS)

Wingett, Paul T. (Inventor); Hanlon, Casey (Inventor)

2017-01-01

An actuator includes a ball nut, a ball screw, and a ball screw stop. The ball nut is adapted to receive an input torque and in response rotates and supplies a drive force. The ball screw extends through the ball nut and has a first end and a second end. The ball screw receives the drive force from the ball nut and in response selectively translates between a retract position and a extend position. The ball screw stop is mounted on the ball screw proximate the first end to translate therewith. The ball screw stop engages the ball nut when the ball screw is in the extend position, translates, with compliance, a predetermined distance toward the first end upon engaging the ball nut, and prevents further rotation of the ball screw upon translating the predetermined distance.

Co-milled API-lactose systems for inhalation therapy: impact of magnesium stearate on physico-chemical stability and aerosolization performance.

PubMed

Lau, Michael; Young, Paul M; Traini, Daniela

2017-06-01

Particle micronization for inhalation can impart surface disorder (amorphism) of crystalline structures. This can lead to stability issues upon storage at elevated humidity from recrystallization of the amorphous state, which can subsequently affect the aerosol performance of the dry powder formulation. The aim of this study was to investigate the impact of an additive, magnesium stearate (MGST), on the stability and aerosol performance of co-milled active pharmaceutical ingredient (API) with lactose. Blends of API-lactose with/without MGST were prepared and co-milled by the jet-mill apparatus. Samples were stored at 50% relative humidity (RH) and 75% RH for 1, 5, and 15 d. Analysis of changes in particle size, agglomerate structure/strength, moisture sorption, and aerosol performance were analyzed by laser diffraction, scanning electron microscopy (SEM), dynamic vapor sorption (DVS), and in-vitro aerodynamic size assessment by impaction. Co-milled formulation with MGST (5% w/w) led to a reduction in agglomerate size and strength after storage at elevated humidity compared with co-milled formulation without MGST, as observed from SEM and laser diffraction. Hysteresis in the sorption/desorption isotherm was observed in the co-milled sample without MGST, which was likely due to the recrystallization of the amorphous regions of micronized lactose. Deterioration in aerosol performance after storage at elevated humidity was greater for the co-milled samples without MGST, compared with co-milled with MGST. MGST has been shown to have a significant impact on co-milled dry powder stability after storage at elevated humidity in terms of physico-chemical properties and aerosol performance.

Use of heat of adsorption to quantify amorphous content in milled pharmaceutical powders.

PubMed

Alam, Shamsul; Omar, Mahmoud; Gaisford, Simon

2014-01-01

Isothermal calorimetry operated in gas perfusion mode (IGPC) is often used to quantify the amorphous content of pharmaceutical powders. Typically, the calibration line is constructed using the heat of crystallisation as the sample is exposed to high levels of a plasticising vapour. However, since the physical form to which the amorphous fraction crystallises may be dependent on the presence of any crystalline seed, the calibration line is often seen to be non-linear, especially as the amorphous content of the sample approaches 100% w/w. Redesigning the experiment so that the calibration line is constructed with the heat of adsorption is an alternative approach that, because it is not dependent upon crystallisation to a physical form should ameliorate this problem. The two methods are compared for a model compound, salbutamol sulphate, which forms either a hydrate or an anhydrate depending on the amorphous content. The heat of adsorption method was linear between amorphous contents of 0 and 100% w/w and resulted in a detection limit of 0.3% w/w and a quantification limit of 0.92% w/w. The heat of crystallisation method was linear only between amorphous contents of 0 and 80% w/w and resulted in a detection limit of 1.7% w/w and a quantification limit of 5.28% w/w. Thus, the use of heat of adsorption is shown to be a better method for quantifying amorphous contents to better than 1% w/w. Copyright © 2013 Elsevier B.V. All rights reserved.

Application of amorphous carbon based materials as antireflective coatings on crystalline silicon solar cells

NASA Astrophysics Data System (ADS)

da Silva, D. S.; Côrtes, A. D. S.; Oliveira, M. H.; Motta, E. F.; Viana, G. A.; Mei, P. R.; Marques, F. C.

2011-08-01

We report on the investigation of the potential application of different forms of amorphous carbon (a-C and a-C:H) as an antireflective coating for crystalline silicon solar cells. Polymeric-like carbon (PLC) and hydrogenated diamond-like carbon films were deposited by plasma enhanced chemical vapor deposition. Tetrahedral amorphous carbon (ta-C) was deposited by the filtered cathodic vacuum arc technique. Those three different amorphous carbon structures were individually applied as single antireflective coatings on conventional (polished and texturized) p-n junction crystalline silicon solar cells. Due to their optical properties, good results were also obtained for double-layer antireflective coatings based on PLC or ta-C films combined with different materials. The results are compared with a conventional tin dioxide (SnO2) single-layer antireflective coating and zinc sulfide/magnesium fluoride (ZnS/MgF2) double-layer antireflective coatings. An increase of 23.7% in the short-circuit current density, Jsc, was obtained using PLC as an antireflective coating and 31.7% was achieved using a double-layer of PLC with a layer of magnesium fluoride (MgF2). An additional increase of 10.8% was obtained in texturized silicon, representing a total increase (texturization + double-layer) of about 40% in the short-circuit current density. The potential use of these materials are critically addressed considering their refractive index, optical bandgap, absorption coefficient, hardness, chemical inertness, and mechanical stability.

Influence of Sn-Mg co-substitution on the microstructural and magnetic characteristics of M-type SrCaLa hexagonal ferrites

NASA Astrophysics Data System (ADS)

Yang, Yujie; Wang, Fanhou; Huang, Duohui; Shao, Juxiang; Tang, Jin; Ur Rehman, Khalid Mehmood; Wu, Zhen

2018-04-01

Sn-Mg co-substituted M-type SrCaLa hexaferrites Sr0.5Ca0.2La0.3Fe12.0-2x(SnMg)xO19 (0.0 ≤ x ≤ 0.5) have been synthesized by ball milling and calcining. The results of X-ray diffraction show that a single magnetoplumbite phase is exhibited in all the samples and no impurity phase is observed in the structure. Lattice constants (c and a) increase with increasing Sn-Mg content (x) from 0.0 to 0.5. Platelet like structure exhibited by FE-SEM micrographs confirms the hexagonal structure of the synthesized samples. The saturation magnetization (Ms) first increases with increasing SnMg content (x) from 0.0 to 0.1, and then decreases when Sn-Mg content (x) ≥ 0.1. The remanent magnetization (Mr), Mr/Ms ratio, coercivity (Hc), magnetic anisotropy field (Ha) and first anisotropy constant (K1) decrease with increasing Sn-Mg content (x) from 0.0 to 0.5.

Spontaneously intermixed Al-Mg barriers enable corrosion-resistant Mg/SiC multilayer coatings

DOE PAGES

Soufli, Regina; Fernandez-Perea, Monica; Baker, Sherry L.; ...

2012-07-24

Magnesium/silicon carbide (Mg/SiC) has the potential to be the best-performing reflective multilayercoating in the 25–80 nm wavelength region but suffers from Mg-related corrosion, an insidious problem which completely degrades reflectance. We have elucidated the origins and mechanisms of corrosion propagation within Mg/SiC multilayers. Based on our findings, we have demonstrated an efficient and simple-to-implement corrosion barrier for Mg/SiC multilayers. In conclusion, the barrier consists of nanometer-scale Mg and Al layers that intermix spontaneously to form a partially amorphous Al-Mg layer and is shown to prevent atmospheric corrosion while maintaining the unique combination of favorable Mg/SiC reflective properties.

Using thermally stimulated current (TSC) to investigate disorder in micronized drug substance produced at different milling energies.

PubMed

Forcino, Rachel; Brum, Jeffrey; Galop, Marc; Sun, Yan

2010-10-01

To investigate the use of thermally stimulated current (TSC) to characterize disorder resulting from micronization of a crystalline drug substance. Samples processed at different milling energies are characterized, and annealing studied. Molecular mobility in micronized drug substance was studied using TSC and compared to results from differential scanning calorimetry (DSC). The micronized drug substance TSC spectra are compared to crystalline and amorphous references. TSC shows distinct relaxation modes for micronized material in comparison to a single weak exotherm observed with DSC. Molecular mobility modes are unique for micronized material compared to the amorphous reference indicating physically distinct disorder compared to phase-separated amorphous material. Signals are ascribed as arising from crystal defects. TSC differentiates material processed at different milling energies showing reasonable correlation between the AUC of the α-relaxation and micronization energy. The annealing process of crystal defects in micronized drug appears to proceed differently for α and β relaxations. TSC proves sensitive to the crystal defects in the micronized drug substance studied here. The technique is able to differentiate distinct types of disorder and can be used to characterize noncrystalline regions arising from milling processes which are physically distinct from amorphous material.

[Amorphous silica. Types, health effects of exposure, NDS].

PubMed

Woźniak, H; Wiecek, E

1995-01-01

Maximum allowable concentration (MAC) values for amorphous silica dust have not been identified in the Polish legal regulations up-to-date. In this work the authors review values of allowable (recommended) amorphous silica dust concentrations in other countries. Data on other types of amorphous silica (natural and synthetic) used in industry as well as data on health effects of exposure to these types of dust are presented. The work encompasses 42 entries in the references and one Table which includes the following proposed MAC values: Non-calcinate diatomaceous earth (diatomite) and synthetic silica: Total dust--10 mg/m3 Respirable dust--2 mg/m3 Calcinate diatomaceous earth (diatomite) and fused silica (vitreous silica): Total dust--2 mg/m3 Respirable dust--1 mg/m3.

5. DETAIL OF ROD MILL BASE AND CONVEYOR BELT SUPPORT, ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

5. DETAIL OF ROD MILL BASE AND CONVEYOR BELT SUPPORT, EAST VIEW. - Vanadium Corporation of America (VCA) Naturita Mill, Grinding Rod Mill, 3 miles Northwest of Naturita, between Highway 141 & San Miguel River, Naturita, Montrose County, CO

Atomic-scale compositional mapping reveals Mg-rich amorphous calcium phosphate in human dental enamel

PubMed Central

La Fontaine, Alexandre; Zavgorodniy, Alexander; Liu, Howgwei; Zheng, Rongkun; Swain, Michael; Cairney, Julie

2016-01-01

Human dental enamel, the hardest tissue in the body, plays a vital role in protecting teeth from wear as a result of daily grinding and chewing as well as from chemical attack. It is well established that the mechanical strength and fatigue resistance of dental enamel are derived from its hierarchical structure, which consists of periodically arranged bundles of hydroxyapatite (HAP) nanowires. However, we do not yet have a full understanding of the in vivo HAP crystallization process that leads to this structure. Mg2+ ions, which are present in many biological systems, regulate HAP crystallization by stabilizing its precursor, amorphous calcium phosphate (ACP), but their atomic-scale distribution within HAP is unknown. We use atom probe tomography to provide the first direct observations of an intergranular Mg-rich ACP phase between the HAP nanowires in mature human dental enamel. We also observe Mg-rich elongated precipitates and pockets of organic material among the HAP nanowires. These observations support the postclassical theory of amelogenesis (that is, enamel formation) and suggest that decay occurs via dissolution of the intergranular phase. This information is also useful for the development of more accurate models to describe the mechanical behavior of teeth. PMID:27617291

Fabrication of micro-lens array on convex surface by meaning of micro-milling

NASA Astrophysics Data System (ADS)

Zhang, Peng; Du, Yunlong; Wang, Bo; Shan, Debin

2014-08-01

In order to develop the application of the micro-milling technology, and to fabricate ultra-precision optical surface with complex microstructure, in this paper, the primary experimental research on micro-milling complex microstructure array is carried out. A complex microstructure array surface with vary parameters is designed, and the mathematic model of the surface is set up and simulated. For the fabrication of the designed microstructure array surface, a micro three-axis ultra-precision milling machine tool is developed, aerostatic guideway drove directly by linear motor is adopted in order to guarantee the enough stiffness of the machine, and novel numerical control strategy with linear encoders of 5nm resolution used as the feedback of the control system is employed to ensure the extremely high motion control accuracy. With the help of CAD/CAM technology, convex micro lens array on convex spherical surface with different scales on material of polyvinyl chloride (PVC) and pure copper is fabricated using micro tungsten carbide ball end milling tool based on the ultra-precision micro-milling machine. Excellent nanometer-level micro-movement performance of the axis is proved by motion control experiment. The fabrication is nearly as the same as the design, the characteristic scale of the microstructure is less than 200μm and the accuracy is better than 1μm. It prove that ultra-precision micro-milling technology based on micro ultra-precision machine tool is a suitable and optional method for micro manufacture of microstructure array surface on different kinds of materials, and with the development of micro milling cutter, ultraprecision micro-milling complex microstructure surface will be achieved in future.

On the decrepitation mechanism of MgNi and LaNi 5-based electrodes studied by in situ acoustic emission

NASA Astrophysics Data System (ADS)

Etiemble, A.; Idrissi, H.; Roué, L.

In situ monitoring of the pulverization of amorphous MgNi and crystalline LaNi 5-based alloys has been studied during their hydrogen charge by combining acoustic emission and electrochemical measurements. In both alloys, two classes of acoustic signals with specific temporal and energetic characteristics were detected during their charge: a P1 class related to the particle cracking and a P2 class due to the release of H 2 bubbles. By comparing the P1 activity on both materials as a function of the charge input, it was shown that the pulverization phenomenon becomes significant at a much lower charge input for the LaNi 5-based electrode (∼5-25 mAh g -1) than for the MgNi electrode (∼365 mAh g -1), reflecting the fact that the mechanism responsible of their decrepitation is not similar. Indeed, it was demonstrated that the cracking of the amorphous and porous MgNi material is mainly induced by the hydrogen evolution reaction whereas for the crystalline and denser LaNi 5-based material, the α-β lattice expansion is responsible of its decrepitation. It was also shown that the particle size and the charge current density have a major impact on the MgNi decrepitation. The correlation between the MgNi particle cracking and the discharge capacity decay with cycling was established.

Carbonate mineralization via an amorphous calcium carbonate (ACC) pathway: Tuning polymorph selection by Mg, pH, and mixing environment

NASA Astrophysics Data System (ADS)

Dove, P. M.; Blue, C.; Mergelsberg, S. T.; Giuffre, A. J.; Han, N.; De Yoreo, J. J.

2017-12-01

Mineral formation by nonclassical processes is widespread with many pathways that include aggregation of nanoparticles, oriented attachment of fully formed crystals, and sequential nucleation/transformation of amorphous phases (De Yoreo et al., 2015, Science). Field observations indicate amorphous calcium carbonate (ACC) can be the initial precipitate when local conditions promote high supersaturations for short time periods. Examples include microbial mats, marine porewaters that undergo pulses of increased alkalinity, closed basin lakes, and sabkhas. The crystalline products exhibit diverse morphologies and complex elemental and isotopic signatures. This study quantifies relationships between solution composition and the crystalline polymorphs that transform from ACC (Blue et al., GCA, 2017). Our experimental design synthesized ACC under controlled conditions for a suite of compositions by tuning input pH, Mg/Ca, and total carbonate concentration. ACC products were allowed to transform within output suspensions under stirred or quiescent mixing while characterizing the polymorph and composition of evolving solutions and solids. We find that ACC transforms to crystalline polymorphs with a systematic relationship to solution composition to give a quantitative framework based upon solution aMg2+/aCa2+ and aCO32-/aCa2+. We also measure a polymorph-specific evolution of pH and Mg/Ca during the transformation that indicates the initial polymorph to form. Pathway is further modulated by stirring versus quiescent conditions. The findings reconcile discrepancies among previous studies of ACC to crystalline products and supports claims that monohydrocalcite may be an overlooked, transient phase during formation of some aragonite and calcite deposits. Organic additives and extreme pH are not required to tune composition and polymorph. Insights from this study reiterate the need to revisit long-standing dogmas regarding controls on CaCO3 polymorph selection. Classical models

Economical drive for large tube mills by means of planetary gears

NASA Technical Reports Server (NTRS)

Ackle, W.

1980-01-01

The performance of heavy-duty planetary gear drives for ball mills used in the cement industry since 1967 is described. These gear drives transmit up to 8500 HP per installation. A reliable method for establishing gear drive efficiency is described and possible savings due to higher efficiency are indicated.

Effect of Milling Time on the Blocking Temperature of Nanoparticles of Magnetocaloric Gd5Si4

NASA Astrophysics Data System (ADS)

Hadimani, Ravi; Gupta, Shalbh; Harstad, Shane; Pecharsky, Vitalij; Jiles, David; David C Jiles Team; Vitalij Pecharsky Collaboration

Extensive research has been done on giant magnetocaloric material Gd5(SixGe1-x)4 to improve adiabatic temperature/isothermal entropy change. However, there have been only a few reports on fabrication of nanostructure/nanoparticles that can be used to tune various properties by changing the length scale. Recently we have reported fabrication of room temperature ferromagnetic nanoparticles of Gd5Si4 using high energy ball milling. These nanoparticles have potential applications in biomedical engineering such as better T2 MRI contrast agents and in hypothermia. Here we report the effect of milling time on the blocking temperature, micro-structure, crystal structure, and magnetic properties of these nanoparticles. Magnetization vs. temperature at an applied field of 100 Oe is measured for all the ball milled samples. Bulk Gd5Si4 has a transition temperature of ~340 K. There are two phase transitions observed in the nanoparticles, one near 300 K corresponding to the Gd5Si4 phase and another between 75-150 K corresponding to Gd5Si3. Zero Field Cooling (ZFC) and Field Cooling (FC) were measured. The blocking temperatures for the nanoparticles increase with decrease in milling time.

Micro sized implantable ball lens-based fiber optic probe design

NASA Astrophysics Data System (ADS)

Cha, Jaepyeong; Kang, Jin U.

2014-02-01

A micro sized implantable ball lens-based fiber optic probe design is described for continuous monitoring of brain activity in freely behaving mice. A prototype uses a 500-micron ball lens and a highly flexible 350-micron-diameter fiber bundle, which are enclosed by a 21G stainless steel sheath. Several types and thickness of brain tissue, consisting of fluorescent probes such as GFP, GCaMP3 calcium indicator, are used to evaluate the performance of the imaging probe. Measured working distance is approximately 400-μm, but is long enough to detect neural activities from cortical and cerebellar tissues of mice brain.

Spin transport and spin accumulation signals in Si studied in tunnel junctions with a Fe/Mg ferromagnetic multilayer and an amorphous SiOxNy tunnel barrier

NASA Astrophysics Data System (ADS)

Nakane, Ryosho; Hada, Takato; Sato, Shoichi; Tanaka, Masaaki

2018-04-01

We studied the spin accumulation signals in phosphorus-doped n+-Si (8 × 1019 cm-3) by measuring the spin transport in three-terminal vertical devices with Fe(3 nm)/Mg(0 and 1 nm)/SiOxNy(1 nm)/n+-Si(001) tunnel junctions, where the amorphous SiOxNy layer was formed by oxnitridation of the Si substrate with radio frequency plasma. Obvious spin accumulation signals were observed at 4-300 K in the spin extraction geometry when the thickness of the Mg insertion layer was 1 nm. We found that by inserting a thin (1 nm) Mg layer, intermixing of Fe and SiOxNy is suppressed, leading to the appearance of the spin accumulation signals, and this result is consistent with the dead layer model recently proposed by our group [S. Sato et al., Appl. Phys. Lett. 107, 032407 (2015)]. We obtained relatively high spin polarization (PS) of electrons tunneling through the junction and long spin lifetime (τS): PS = 16% and τS = 5.6 ns at 4 K and PS = 7.5% and τS = 2.7 ns at 300 K. Tunnel junctions with an amorphous SiOxNy tunnel barrier are very promising for Si-based spintronic devices, since they can be formed by the method compatible with the silicon complementary metal-oxide-semiconductor technology.

Ball Powder Production Wastewater Biodegradation Support Studies - With Nitroglycerine

DTIC Science & Technology

1989-02-01

in the wastewater. Characterization of the ball powder wastewater stream showed an actual average NG inlet concentration of 192 mg/L. Pilot test...the first phase of pilot testing, the recommendation was made to conduct an additional pilot test phase to determine the effect of nitroglycerin (NG...NG by aerobic bacteria, a pilot program was undertaken with the following objectives: 1) to determine the concentration of NG in the ball powder

Friction and wear performance of bearing ball sliding against diamond-like carbon coatings

NASA Astrophysics Data System (ADS)

Wu, Shenjiang; Kousaka, Hiroyuki; Kar, Satyananda; Li, Dangjuan; Su, Junhong

2017-01-01

We have studied the tribological properties of bearing steel ball (Japan standard, SUJ2) sliding against tetrahedral amorphous carbon (ta-C) coatings and amorphous hydrogenated carbon (a-C:H) coatings. The reciprocating sliding testes are performed with ball-on-plate friction tester in ambient air condition. Analysis of friction coefficient, wear volume and microstructure in wear scar are carried out using optical microscopy, atom force morphology (AFM) and Raman spectroscopy. The results show the SUJ2 on ta-C coating has low friction coefficient (around 0.15) but high wear loss. In contrast, the low wear loss of SUJ2 on a-C:H coating with high (around 0.4) and unsteady friction coefficient. Some Fe2O3, FeO and graphitization have been found on the wear scar of SUJ2 sliding against ta-C coating. Nearly no oxide materials exist on the wear scar of SUJ2 against a-C:H coating. The mechanism and hypothesis of the wear behavior have been investigated according to the measurement results. This study will contribute to proper selection and understand the tribological performance of bearing steels against DLC coatings.

Corrosion-Resistant Ball Bearings

NASA Technical Reports Server (NTRS)

Zdankiewicz, E. M.; Linaburg, E. L.; Lytle, L. J.

1990-01-01

Self-lubricating bearing system withstands highly corrosive environment of wastewater-recycling unit. New bearings contain cobalt-based-alloy balls and races, graphite/polyimide polymer ball cages, and single integral polytetrafluoroethylene seals on wet sides. Materials and design prevent corrosion by acids and provide lubrication.

Enhanced hydrogen sorption kinetics of Mg 50Ni-LiBH 4 composite by CeCl 3 addition

NASA Astrophysics Data System (ADS)

Gennari, F. C.; Puszkiel, J. A.

Mg 50Ni-LiBH 4 and Mg 50Ni-LiBH 4-CeCl 3 composites have been prepared by short times of ball milling under argon atmosphere. Combination of HP-DSC and volumetric techniques show that Mg 50Ni-LiBH 4-CeCl 3 composite not only uptakes hydrogen faster than Mg 50Ni-LiBH 4, but also releases hydrogen at a lower temperature (225 °C). The presence of CeCl 3 has a catalytic role, but it does not modify the thermodynamic properties of the composite which corresponds to MgH 2. Experimental studies on the hydriding/dehydriding mechanisms demonstrate that LiBH 4 and Ni lead to the formation of MgNi 3B 2 in both composites. In addition, XRD/DSC analysis and thermodynamic calculations demonstrate that the addition of CeCl 3 accounts for the enhancement of the hydrogen absorption/desorption kinetics through the interaction with LiBH 4. The in situ formation and subsequent decomposition of Ce(BH 4) 3 provides a uniform distribution of nanosize CeB 4 compound, which plays an important role in improving the kinetic properties of MgH 2.

Modeling the milling tool wear by using an evolutionary SVM-based model from milling runs experimental data

NASA Astrophysics Data System (ADS)

Nieto, Paulino José García; García-Gonzalo, Esperanza; Vilán, José Antonio Vilán; Robleda, Abraham Segade

2015-12-01

The main aim of this research work is to build a new practical hybrid regression model to predict the milling tool wear in a regular cut as well as entry cut and exit cut of a milling tool. The model was based on Particle Swarm Optimization (PSO) in combination with support vector machines (SVMs). This optimization mechanism involved kernel parameter setting in the SVM training procedure, which significantly influences the regression accuracy. Bearing this in mind, a PSO-SVM-based model, which is based on the statistical learning theory, was successfully used here to predict the milling tool flank wear (output variable) as a function of the following input variables: the time duration of experiment, depth of cut, feed, type of material, etc. To accomplish the objective of this study, the experimental dataset represents experiments from runs on a milling machine under various operating conditions. In this way, data sampled by three different types of sensors (acoustic emission sensor, vibration sensor and current sensor) were acquired at several positions. A second aim is to determine the factors with the greatest bearing on the milling tool flank wear with a view to proposing milling machine's improvements. Firstly, this hybrid PSO-SVM-based regression model captures the main perception of statistical learning theory in order to obtain a good prediction of the dependence among the flank wear (output variable) and input variables (time, depth of cut, feed, etc.). Indeed, regression with optimal hyperparameters was performed and a determination coefficient of 0.95 was obtained. The agreement of this model with experimental data confirmed its good performance. Secondly, the main advantages of this PSO-SVM-based model are its capacity to produce a simple, easy-to-interpret model, its ability to estimate the contributions of the input variables, and its computational efficiency. Finally, the main conclusions of this study are exposed.

Comparative Studies on Al-Based Composite Powder Reinforced with Nano Garnet and Multi-wall Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Basariya, M. Raviathul; Srivastava, V. C.; Mukhopadhyay, N. K.

2015-11-01

Effect of mechanical alloying/milling on microstructural evolution and hardness variations of garnet and multi-walled carbon nanotubes (MWCNTs)-reinforced Al-Mg-Si alloy (EN AW6082) composites are investigated. Structural and morphological studies revealed that the composite powders prepared by milling display a more homogenous distribution of the reinforcing particles. Improved nanoindentation hardness viz., 4.24 and 5.90 GPa are achieved for EN AW6082/Garnet and EN AW6082/MWCNTs composites, respectively, and it is attributed to severe deformation of the aluminum alloy powders and embedding of the harder reinforcement particles uniformly into the aluminum alloy matrix. However, enhancement in case of MWCNTs-reinforced composite makes apparent the effect of its nanosized uniform dispersion in the matrix, thereby resisting the plastic deformation at lower stress and increased dislocation density evolved during high-energy ball milling. The results of the present study indicate that carbon nanotubes and garnet can be effectively used as reinforcements for Al-based composites.

Processing and characterization of Zr-based metallic glass by laser direct deposition

NASA Astrophysics Data System (ADS)

Bae, Heehun

Bulk Metallic Glass has become famous for its exceptional mechanical and corrosion properties. Especially, Zirconium has been the prominent constituent in Bulk Metallic Glass due to its superior glass forming ability, the ability to form amorphous phase with low cooling rate, thereby giving advantages in structural applications. In this study, Zirconium powder was alloyed with Aluminum, Nickel and Copper powder at an atomic ratio of 65:10:10:15, respectively. Using the ball milling process to mix the powders, Zr65Al10Ni 10Cu15 amorphous structure was manufactured by laser direct deposition. Laser power and laser scanning speed were optimized to increase the fraction of amorphous phase. X-ray Diffraction confirmed the existence of both amorphous and crystalline phase by having a wide halo peak and sharp intense peak in the spectrum. Differential Scanning Calorimetry proved the presence of amorphous phase and glass transition was observed to be around 655 K. Scanning electron microscopy showed the microstructure of the deposited sample to have repetitive amorphous and crystalline phase as XRD examined. Crystalline phase resulted from the laser reheating and remelting process due to subsequent laser scan. Laser direct deposited amorphous/crystalline composite showed Vickers Hardness of 670 Hv and exhibited improved corrosion resistance in comparison to fully-crystallized sample. The compression test showed that, due to the existence of crystalline phase, fracture strain of Zr65Al10Ni10Cu 15 amorphous composites was enhanced from less than 2% to as high as 5.7%, compared with fully amorphous metallic glass.

Apparatus and method for inspecting a bearing ball

NASA Technical Reports Server (NTRS)

Bankston, B. F. (Inventor)

1985-01-01

A method and apparatus for inspecting the surface of a ball bearing is disclosed which includes a base having a high friction non-abrasive base scanning surface. A holding device includes a cone-shaped cup recess in which a ball element is received. Air is introduced through a passage to relieve friction between the wall of the recess and the ball element and facilitate rolling of the ball over the high friction base surface. The holding device is moved over the base scanning surface in a predetermined pattern such that the entire surface of the ball element is inspected byan eddy current probe which detects any surface defects.

OVERVIEW OF STAMP MILL SITE,LOOKING SOUTHWEST. THE LOWER TRAM TERMINAL ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

OVERVIEW OF STAMP MILL SITE,LOOKING SOUTHWEST. THE LOWER TRAM TERMINAL IS OUT OF FRAME, JUST TO THE RIGHT. WATER TANK, LOADING PLATFORM, AND TRAM TRESTLE LEADING UP TO THE TRAM TERMINAL ARE AT RIGHT. THE STRUCTURE AT EXTREME RIGHT BELOW THE TRESTLE, ARE REMAINS OF A SECONDARY ORE BIN, WITH BALL MILL FOUNDATIONS AND WOOD DEBRIS JUST BELOW ON THE SECOND LEVEL. AT CENTER IS A BOILER AND THE FRAME WORK OF A FILTER PRESS. THE SMALL STRUCTURE AT CENTER LEFT IS AN INTERPRETIVE SIGN PLACED BY THE PARK SERVICE. AT LOWER LEFT, THIRD LEVEL OF THE MILL, ARE THE REMAINS OF A BLACKSMITH'S FORGE. - Keane Wonder Mine, Park Route 4 (Daylight Pass Cutoff), Death Valley Junction, Inyo County, CA

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chater, R., E-mail: chatersamy@yahoo.fr; Bououdina, M., E-mail: mboudina@gmail.com; Department of Physics, College of Science, University of Bahrain, PO Box 32038, Kingdom of Bahrain

2013-05-01

Nanocrystalline Fe{sub 1–x–y}Ni xCr 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 wellmore » 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.« less

Mechanical ball-milling preparation of fullerene/cobalt core/shell nanocomposites with high electrochemical hydrogen storage ability.

PubMed

Bao, Di; Gao, Peng; Shen, Xiande; Chang, Cheng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Zhou, Xiaoming; Sun, Shuchao; Li, Guobao; Yang, Piaoping

2014-02-26

The design and synthesis of new hydrogen storage nanomaterials with high capacity at low cost is extremely desirable but remains challenging for today's development of hydrogen economy. Because of the special honeycomb structures and excellent physical and chemical characters, fullerenes have been extensively considered as ideal materials for hydrogen storage materials. To take the most advantage of its distinctive symmetrical carbon cage structure, we have uniformly coated C60's surface with metal cobalt in nanoscale to form a core/shell structure through a simple ball-milling process in this work. The X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectra, high-solution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDX) elemental mappings, and X-ray photoelectron spectroscopy (XPS) measurements have been conducted to evaluate the size and the composition of the composites. In addition, the blue shift of C60 pentagonal pinch mode demonstrates the formation of Co-C chemical bond, and which enhances the stability of the as-obtained nanocomposites. And their electrochemical experimental results demonstrate that the as-obtained C60/Co composites have excellent electrochemical hydrogen storage cycle reversibility and considerably high hydrogen storage capacities of 907 mAh/g (3.32 wt % hydrogen) under room temperature and ambient pressure, which is very close to the theoretical hydrogen storage capacities of individual metal Co (3.33 wt % hydrogen). Furthermore, their hydrogen storage processes and the mechanism have also been investigated, in which the quasi-reversible C60/Co↔C60/Co-Hx reaction is the dominant cycle process.

Fabrication of superconducting MgB2 nanostructures by an electron beam lithography-based technique

NASA Astrophysics Data System (ADS)

Portesi, C.; Borini, S.; Amato, G.; Monticone, E.

2006-03-01

In this work, we present the results obtained in fabrication and characterization of magnesium diboride nanowires realized by an electron beam lithography (EBL)-based method. For fabricating MgB2 thin films, an all in situ technique has been used, based on the coevaporation of B and Mg by means of an e-gun and a resistive heater, respectively. Since the high temperatures required for the fabrication of good quality MgB2 thin films do not allow the nanostructuring approach based on the lift-off technique, we structured the samples combining EBL, optical lithography, and Ar milling. In this way, reproducible nanowires 1 μm long have been obtained. To illustrate the impact of the MgB2 film processing on its superconducting properties, we measured the temperature dependence of the resistance on a nanowire and compared it to the original magnesium diboride film. The electrical properties of the films are not degraded as a consequence of the nanostructuring process, so that superconducting nanodevices may be obtained by this method.

The effect of milling time and sintering temperature on Mn, Ti substituted barium hexaferrite nanoparticle

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Manaf, Azwar

2018-04-01

Barium hexaferrite (BaO.6Fe2O3/BaFe12O19) is a permanent magnetic material and microwave absorbing material. The value of microwave absorption can be increased through the engineering of the material structure, while the reduction of crystallite and particle size up to nanometer results device performance improvement to be superior. In this research, the structural engineering through mechanical alloying and crystallite size reduction through high power ultrasonic irradiation will be explained. Mixing and alloying of Sigma Aldrich BaCO3, Fe2O3, MnCO3, TiO2 p.a 99% precursor material used ball mill with powder ratio of vial at 1:10. Mechanical alloying for 60 hours at 160 rpm produced amorphous material. The process of the crystalline embryo nucleation for 4 hours produced multicrystalline material at a sinter temperature of 1100°C. Phase analysis of the mechanical alloying result using x-ray diffractometer was confirmed either the formation of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) single phase. Multicrystalline powder of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) was obtained through 20 hours hand grinding and re-milling to bulk sample. Crystallite size reduction in the analysis was conducted through particle density variation in ultrasonic reactor and variation of the increase in ultrasonic time. Increase in milling time up to 60 hours produced fragmenting so that particle size reduction from 18.8 µm to 0.9 µm was occurred. The 12-h ultrasonic irradiation at a frequency of 20 kHz amplitude of 60 µm produced a crystallite-size reduction up to 18 nm at a 10 g/L particle density.

Pretreatment of eucalyptus wood chips for enzymatic saccharification using combined sulfuric acid-free ethanol cooking and ball milling.

PubMed

Teramoto, Yoshikuni; Tanaka, Noriko; Lee, Seung-Hwan; Endo, Takashi

2008-01-01

A combined sulfuric acid-free ethanol cooking and pulverization process was developed in order to achieve the complete saccharification of the cellulosic component of woody biomass, thereby avoiding the problems associated with the use of strong acid catalysts. Eucalyptus wood chips were used as a raw material and exposed to an ethanol/water/acetic acid mixed solvent in an autoclave. This process can cause the fibrillation of wood chips. During the process, the production of furfural due to an excessive degradation of polysaccharide components was extremely low and delignification was insignificant. Therefore, the cooking process is regarded not as a delignification but as an activation of the original wood. Subsequently, the activated solid products were pulverized by ball-milling in order to improve their enzymatic digestibility. Enzymatic hydrolysis experiments demonstrated that the conversion of the cellulosic components into glucose attained 100% under optimal conditions. Wide-angle X-ray diffractometry and particle size distribution analysis revealed that the scale affecting the improvement of enzymatic digestibility ranged from 10 nm to 1 microm. Field emission scanning electron microscopy depicted that the sulfuric acid-free ethanol cooking induced a pore formation by the removal of part of the lignin and hemicellulose fractions in the size range from a few of tens nanometers to several hundred nanometers. (c) 2007 Wiley Periodicals, Inc.

Research on defects inspection of solder balls based on eddy current pulsed thermography.

PubMed

Zhou, Xiuyun; Zhou, Jinlong; Tian, Guiyun; Wang, Yizhe

2015-10-13

In order to solve tiny defect detection for solder balls in high-density flip-chip, this paper proposed feasibility study on the effect of detectability as well as classification based on eddy current pulsed thermography (ECPT). Specifically, numerical analysis of 3D finite element inductive heat model is generated to investigate disturbance on the temperature field for different kind of defects such as cracks, voids, etc. The temperature variation between defective and non-defective solder balls is monitored for defects identification and classification. Finally, experimental study is carried on the diameter 1mm tiny solder balls by using ECPT and verify the efficacy of the technique.

A Steel Ball Surface Quality Inspection Method Based on a Circumferential Eddy Current Array Sensor.

PubMed

Zhang, Huayu; Xie, Fengqin; Cao, Maoyong; Zhong, Mingming

2017-07-01

To efficiently inspect surface defects on steel ball bearings, a new method based on a circumferential eddy current array (CECA) sensor was proposed here. The best probe configuration, in terms of the coil quality factor (Q-factor), magnetic field intensity, and induced eddy current density on the surface of a sample steel ball, was determined using 3-, 4-, 5-, and 6-coil probes, for analysis and comparison. The optimal lift-off from the measured steel ball, the number of probe coils, and the frequency of excitation current suitable for steel ball inspection were obtained. Using the resulting CECA sensor to inspect 46,126 steel balls showed a miss rate of ~0.02%. The sensor was inspected for surface defects as small as 0.05 mm in width and 0.1 mm in depth.

High Purity and Yield of Boron Nitride Nanotubes Using Amorphous Boron and a Nozzle-Type Reactor

PubMed Central

Kim, Jaewoo; Seo, Duckbong; Yoo, Jeseung; Jeong, Wanseop; Seo, Young-Soo; Kim, Jaeyong

2014-01-01

Enhancement of the production yield of boron nitride nanotubes (BNNTs) with high purity was achieved using an amorphous boron-based precursor and a nozzle-type reactor. Use of a mixture of amorphous boron and Fe decreases the milling time for the preparation of the precursor for BNNTs synthesis, as well as the Fe impurity contained in the B/Fe interdiffused precursor nanoparticles by using a simple purification process. We also explored a nozzle-type reactor that increased the production yield of BNNTs compared to a conventional flow-through reactor. By using a nozzle-type reactor with amorphous boron-based precursor, the weight of the BNNTs sample after annealing was increased as much as 2.5-times with much less impurities compared to the case for the flow-through reactor with the crystalline boron-based precursor. Under the same experimental conditions, the yield and quantity of BNNTs were estimated as much as ~70% and ~1.15 g/batch for the former, while they are ~54% and 0.78 g/batch for the latter. PMID:28788161

High Purity and Yield of Boron Nitride Nanotubes Using Amorphous Boron and a Nozzle-Type Reactor.

PubMed

Kim, Jaewoo; Seo, Duckbong; Yoo, Jeseung; Jeong, Wanseop; Seo, Young-Soo; Kim, Jaeyong

2014-08-11

Enhancement of the production yield of boron nitride nanotubes (BNNTs) with high purity was achieved using an amorphous boron-based precursor and a nozzle-type reactor. Use of a mixture of amorphous boron and Fe decreases the milling time for the preparation of the precursor for BNNTs synthesis, as well as the Fe impurity contained in the B/Fe interdiffused precursor nanoparticles by using a simple purification process. We also explored a nozzle-type reactor that increased the production yield of BNNTs compared to a conventional flow-through reactor. By using a nozzle-type reactor with amorphous boron-based precursor, the weight of the BNNTs sample after annealing was increased as much as 2.5-times with much less impurities compared to the case for the flow-through reactor with the crystalline boron-based precursor. Under the same experimental conditions, the yield and quantity of BNNTs were estimated as much as ~70% and ~1.15 g/batch for the former, while they are ~54% and 0.78 g/batch for the latter.

A real-time surface inspection system for precision steel balls based on machine vision

NASA Astrophysics Data System (ADS)

Chen, Yi-Ji; Tsai, Jhy-Cherng; Hsu, Ya-Chen

2016-07-01

Precision steel balls are one of the most fundament components for motion and power transmission parts and they are widely used in industrial machinery and the automotive industry. As precision balls are crucial for the quality of these products, there is an urgent need to develop a fast and robust system for inspecting defects of precision steel balls. In this paper, a real-time system for inspecting surface defects of precision steel balls is developed based on machine vision. The developed system integrates a dual-lighting system, an unfolding mechanism and inspection algorithms for real-time signal processing and defect detection. The developed system is tested under feeding speeds of 4 pcs s-1 with a detection rate of 99.94% and an error rate of 0.10%. The minimum detectable surface flaw area is 0.01 mm2, which meets the requirement for inspecting ISO grade 100 precision steel balls.

Preparation and characterization of mechanically alloyed AB3-type based material LaMg2Ni5Al4 and its solid-gaz hydrogen storage reaction

NASA Astrophysics Data System (ADS)

Jaafar, Hassen; Aymard, Luc; Dachraoui, Walid; Demortière, Arnaud; Abdellaoui, Mohieddine

2018-04-01

We developed in the present paper the synthesis of a new AB3-type compound LaMg2Ni5Al4 by mechanical alloying (MA) process. ​​X-ray diffraction analysis (XRD) was used to determine the structural properties and the phase evolution of the powder mixtures. Two different synthesis pathways have been investigated. The first starting from elemental metals and the second from a mixture of two binary compounds LaNi5 (CaCu5-type structure, P6/mmm space group) and Al(Mg) solid solution (cubic Fm-3 m space group). The results show multiphase alloys which contain LaMg2Ni5Al4 main phase with hexagonal PuNi3-type structure (R-3 m space group). Rietveld analysis shows that using a planetary ball mill, we obtain a good yield of LaMg2Ni5Al4 compound after 5 h of mechanical alloying for both synthesis pathways. TEM analysis confirmed XRD results. SEM-EDX analysis of the final product was in agreement with the nominal chemical formula. A setup of possible solid-gaz hydrogenation reaction will be described so far at the end of this work. Electrochemical results demonstrate evidence on hydrogen absorption in the AB3 material and the discharge capacity was equal to 5.9 H/f.u.

Polyurethane retainers for ball bearings

NASA Technical Reports Server (NTRS)

Christy, R. I.

1973-01-01

Evaluation of a new ball bearing retainer material is reported. A special composite polyurethane foam ball retainer has been developed that has virtually zero wear, is chemically inert to hydrocarbon lubricants, and stores up to 60 times as much lubricant per unit volume as the most commonly used retainer material, cotton phenolic. This new retainer concept shows promise of years of ball bearing operation without reoiling, based on life testing in high vacuum.

Stacking faults and mechanisms strain-induced transformations of hcp metals (Ti, Mg) during mechanical activation in liquid hydrocarbons

NASA Astrophysics Data System (ADS)

Lubnin, A. N.; Dorofeev, G. A.; Nikonova, R. M.; Mukhgalin, V. V.; Lad'yanov, V. I.

2017-11-01

The evolution of the structure and substructure of metals Ti and Mg with hexagonal close-packed (hcp) lattice is studied during their mechanical activation in a planetary ball mill in liquid hydrocarbons (toluene, n-heptane) and with additions of carbon materials (graphite, fullerite, nanotubes) by X-ray diffraction, scanning electron microscopy, and chemical analysis. The temperature behavior and hydrogen-accumulating properties of mechanocomposites are studied. During mechanical activation of Ti and Mg, liquid hydrocarbons decay, metastable nanocrystalline titanium carbohydride Ti(C,H) x and magnesium hydride β-MgH2 are formed, respectively. The Ti(C,H) x and MgH2 formation mechanisms during mechanical activation are deformation ones and are associated with stacking faults accumulation, and the formation of face-centered cubic (fcc) packing of atoms. Metastable Ti(C,H)x decays at a temperature of 550°C, the partial reverse transformation fcc → hcp occurs. The crystalline defect accumulation (nanograin boundaries, stacking faults), hydrocarbon destruction, and mechanocomposite formation leads to the enhancement of subsequent magnesium hydrogenation in the Sieverts reactor.

10. RW Meyer Sugar Mill: 18761889. Simple, singlecylinder, horizontal, reciprocating ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

10. RW Meyer Sugar Mill: 1876-1889. Simple, single-cylinder, horizontal, reciprocating steam engine, model No. 1, 5' x 10', 6 hp, 175 rpm. Manufactured by Ames Iron Works, Oswego, New York, 1879. View: Steam engine powered the mill's centrifugals. To the left of the horizontal (fluted) cylinder is the water pump which moved the boiler feed water through the engine's pre-heat system (the exhaust steam heated the boiler feedwater before it was pumped on to the boiler). The steam-feed port, manual throttle valve, and fly-ball governor and pulley and to the right of the cylinder. The drive shaft with flywheel to the left and pulley to the right are seen behind the piston rod, cross-head, wrist pen, connecting rod and the slide valve and eccentric. - R. W. Meyer Sugar Mill, State Route 47, Kualapuu, Maui County, HI

Miniature ball-tip optical fibers for use in thulium fiber laser ablation of kidney stones

NASA Astrophysics Data System (ADS)

Wilson, Christopher R.; Hardy, Luke A.; Kennedy, Joshua D.; Irby, Pierce B.; Fried, Nathaniel M.

2016-01-01

Optical fibers, consisting of 240-μm-core trunk fibers with rounded, 450-μm-diameter ball tips, are currently used during Holmium:YAG laser lithotripsy to reduce mechanical damage to the inner lining of the ureteroscope working channel during fiber insertion and prolong ureteroscope lifetime. Similarly, this study tests a smaller, 100-μm-core fiber with 300-μm-diameter ball tip during thulium fiber laser (TFL) lithotripsy. TFL was operated at a wavelength of 1908 nm, with 35-mJ pulse energy, 500-μs pulse duration, and 300-Hz pulse rate. Calcium oxalate/phosphate stone samples were weighed, laser procedure times were measured, and ablation rates were calculated for ball tip fibers, with comparison to bare tip fibers. Photographs of ball tips were taken before and after each procedure to track ball tip degradation and determine number of procedures completed before need for replacement. A high speed camera also recorded the cavitation bubble dynamics during TFL lithotripsy. Additionally, saline irrigation rates and ureteroscope deflection were measured with and without the presence of TFL fiber. There was no statistical difference (P>0.05) between stone ablation rates for single-use ball tip fiber (1.3±0.4 mg/s) (n=10), multiple-use ball tip fiber (1.3±0.5 mg/s) (n=44), and conventional single-use bare tip fibers (1.3±0.2 mg/s) (n=10). Ball tip durability varied widely, but fibers averaged greater than four stone procedures before failure, defined by rapid decline in stone ablation rates. Mechanical damage at the front surface of the ball tip was the limiting factor in fiber lifetime. The small fiber diameter did not significantly impact ureteroscope deflection or saline flow rates. The miniature ball tip fiber may provide a cost-effective design for safe fiber insertion through the ureteroscope working channel and into the ureter without risk of instrument damage or tissue perforation, and without compromising stone ablation efficiency during TFL lithotripsy.

The effect of milling frequency on a mechanochemical organic reaction monitored by in situ Raman spectroscopy

PubMed Central

Julien, Patrick A; Malvestiti, Ivani

2017-01-01

We provide the first in situ and real-time study of the effect of milling frequency on the course of a mechanochemical organic reaction conducted using a vibratory shaker (mixer) ball mill. The use of in situ Raman spectroscopy for real-time monitoring of the mechanochemical synthesis of a 2,3-diphenylquinoxaline derivative revealed a pronounced dependence of chemical reactivity on small variations in milling frequency. In particular, in situ measurements revealed the establishment of two different regimes of reaction kinetics at different frequencies, providing tentative insight into processes of mechanical activation in organic mechanochemical synthesis. PMID:29114323

Ball clay

USGS Publications Warehouse

Virta, R.L.

2001-01-01

Part of the 2000 annual review of the industrial minerals sector. A general overview of the ball clay industry is provided. In 2000, sales of ball clay reached record levels, with sanitary ware and tile applications accounting for the largest sales. Ball clay production, consumption, prices, foreign trade, and industry news are summarized. The outlook for the ball clay industry is also outlined.

Degradation of trichloroethene with a noval ball milled Fe-C nanocomposite

DOE PAGES

Gao, Jie; Wang, Wei; Rondinone, Adam Justin; ...

2015-07-18

Nanoscale zero-valent iron (NZVI) is effective in reductively degrading dense non-aqueous phase liquids (DNAPLs), such as trichloroethene (TCE), in groundwater (i.e., dechlorination) although the NZVI technology itself still suffers from high material costs and inability to target hydrophobic contaminants in source zones. To address these problems, we developed a novel, inexpensive iron-carbon (Fe-C) nanocomposite material by simultaneously milling micron-size iron and activated carbon powder. Microscopic and X-ray diffraction (XRD) characterization of the composite material revealed that nanoparticles of Fe were dispersed in activated carbon and a new iron carbide phase was formed. Bench-scale studies showed that this material instantaneously sorbedmore » >90% of TCE from aqueous solutions and subsequently decomposed TCE into non-chlorinated products. Compared to milled Fe, Fe-C nanocomposite dechlorinated TCE at a slightly slower rate and favored the production of ethene over other TCE degradation products such as C 3-C 6 compounds. When placed in hexane-water mixture, the Fe-C nanocomposite materials are preferentially partitioned into the organic phase, indicating the ability of the composite materials to target DNAPL during remediation.« less

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals.

PubMed

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-07-05

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites.

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals

PubMed Central

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P.; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-01-01

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites. PMID:27378145

The synthesis of Cu/Fe/Fe3O4 catalyst through the aqueous solution ball milling method assisted by high-frequency electromagnetic field

NASA Astrophysics Data System (ADS)

Yingzhe, Zhang; Yuxing, He; Qingdong, Qin; Fuchun, Wang; Wankun, Wang; Yongmei, Luo

2018-06-01

In this paper, nano-magnetic Cu/Fe/Fe3O4 catalyst was prepared by a new aqueous solution ball milling method assisted by high-frequency electromagnetic field at room temperature. The products were characterized by means of X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED), and vibrating sample magnetometer (VSM). Microwave induced catalytic degradation of methylene blue (MB) was carried out in the presence of Cu/Fe/Fe3O4. The concentration of methylene blue was determined by UV-Vis spectrophotometry. The solid catalyst showed high catalytic activity of degrade MB and considerable saturation magnetization, lower remanence and coercivity. It indicate that the catalyst can be effectively separated for reuse by simply applying an external magnetic field and it can greatly promote their potential industrial application to eliminate organic pollutants from waste-water. Finally, we found that it is the non-thermal effect of microwave that activated the catalytic activity of Cu/Fe/Fe3O4 to degrade MB.

Calorimetry investigations of milled α-tricalcium phosphate (α-TCP) powders to determine the formation enthalpies of α-TCP and X-ray amorphous tricalcium phosphate.

PubMed

Hurle, Katrin; Neubauer, Juergen; Bohner, Marc; Doebelin, Nicola; Goetz-Neunhoeffer, Friedlinde

2015-09-01

One α-tricalcium phosphate (α-TCP) powder was either calcined at 500°C to obtain fully crystalline α-TCP or milled for different durations to obtain α-TCP powders containing various amounts of X-ray amorphous tricalcium phosphate (ATCP). These powders containing between 0 and 71wt.% ATCP and up to 2.0±0.1wt.% β-TCP as minor phase were then hydrated in 0.1M Na2HPO4 aqueous solution and the resulting heat flows were measured by isothermal calorimetry. Additionally, the evolution of the phase composition during hydration was determined by in situ XRD combined with the G-factor method, an external standard method which facilitates the indirect quantification of amorphous phases. Maximum ATCP hydration was reached after about 1h, while that of crystalline α-TCP hydration occurred between 4 and 11h, depending on the ATCP content. An enthalpy of formation of -4065±6kJ/mol (T=23°C) was calculated for ATCP (Ca3(PO4)2), while for crystalline α-TCP (α-Ca3(PO4)2) a value of -4113±6kJ/mol (T=23°C) was determined. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Cereal-based biorefinery development: utilisation of wheat milling by-products for the production of succinic acid.

PubMed

Dorado, M Pilar; Lin, Sze Ki Carol; Koutinas, Apostolis; Du, Chenyu; Wang, Ruohang; Webb, Colin

2009-08-10

A novel wheat-based bioprocess for the production of a nutrient-complete feedstock for the fermentative succinic acid production by Actinobacillus succinogenes has been developed. Wheat was fractionated into bran, middlings and flour. The bran fraction, which would normally be a waste product of the wheat milling industry, was used as the sole medium in two solid-state fermentations (SSF) of Aspergillus awamori and Aspergillus oryzae that produce enzyme complexes rich in amylolytic and proteolytic enzymes, respectively. The resulting fermentation solids were then used as crude enzyme sources, by adding directly to an aqueous suspension of milled bran and middlings fractions (wheat flour milling by-products) to generate a hydrolysate containing over 95g/L glucose, 25g/L maltose and 300mg/L free amino nitrogen (FAN). This hydrolysate was then used as the sole medium for A. succinogenes fermentations, which led to the production of 50.6g/L succinic acid. Supplementation of the medium with yeast extract did not significantly improve succinic acid production though increasing the inoculum concentration to 20% did result in the production of 62.1g/L succinic acid. Results indicated that A. succinogenes cells were able to utilise glucose and maltose in the wheat hydrolysate for cell growth and succinic acid production. The proposed process could be potentially integrated into a wheat-milling process to upgrade the wheat flour milling by-products (WFMB) into succinic acid, one of the future platform chemicals of a sustainable chemical industry.

Reexamination of Ball-Race Conformity Effects on Ball Bearing Life

NASA Technical Reports Server (NTRS)

Zaretsky, Erwin V.; Poplawski, Joseph V.; Root, Lawrence E.

2007-01-01

The analysis in this report considers the life of the ball set as well as the respective lives of the races to reassess the effect of ball-race conformity on ball bearing life. The related changes in ball bearing life are incorporated in life factors that can be used to modify the bearing predicted life using the Lundberg-Palmgren equations and the ANSI/ABMA and ISO Standards. Two simple algebraic relationships were established to calculate life factors LF(sub c) to determine the effect of inner- and outer-race conformity combinations on bearing L(sub 10) life for deepgroove and angular-contact ball bearings, respectively. Depending on the bearing type and series as well as conformity combinations, the calculated life for deep-groove ball bearings can be over 40 percent less than that calculated by the Lundberg-Palmgren equations. For angular-contact ball bearings, the life can vary between +16 and -39 percent from that calculated by the Lundberg-Palmgren equations. Comparing the two ball bearing types, the life factors LF(sub c) for the deep-groove bearings can be as much as 40 percent lower than that for angular-contact ball bearings.

Amorphous-amorphous transition in a porous coordination polymer.

PubMed

Ohtsu, Hiroyoshi; Bennett, Thomas D; Kojima, Tatsuhiro; Keen, David A; Niwa, Yasuhiro; Kawano, Masaki

2017-07-04

The amorphous state plays a key role in porous coordination polymer and metal-organic framework phase transitions. We investigate a crystalline-to-amorphous-to-amorphous-to-crystalline (CAAC) phase transition in a Zn based coordination polymer, by X-ray absorption fine structure (XAFS) and X-ray pair distribution function (PDF) analysis. We show that the system shows two distinct amorphous phases upon heating. The first involves a reversible transition to a desolvated form of the original network, followed by an irreversible transition to an intermediate phase which has elongated Zn-I bonds.

A novel AFM-based 5-axis nanoscale machine tool for fabrication of nanostructures on a micro ball

NASA Astrophysics Data System (ADS)

Geng, Yanquan; Wang, Yuzhang; Yan, Yongda; Zhao, Xuesen

2017-11-01

This paper presents a novel atomic force microscopy (AFM)-based 5-axis nanoscale machine tool developed to fabricate nanostructures on different annuli of the micro ball. Different nanostructures can be obtained by combining the scratching trajectory of the AFM tip with the movement of the high precision air-bearing spindle. The center of the micro ball is aligned to be coincided with the gyration center of the high precision to guarantee the machining process during the rotating of the air-bearing spindle. Processing on different annuli of the micro ball is achieved by controlling the distance between the center of the micro ball and the rotation center of the AFM head. Nanostructures including square cavities, circular cavities, triangular cavities, and an annular nanochannel are machined successfully on the three different circumferences of a micro ball with a diameter of 1500 μm. Moreover, the influences of the error motions of the high precision air-bearing spindle and the eccentric between the micro ball and the gyration center of the high precision air-bearing spindle on the processing position error on the micro ball are also investigated. This proposed machining method has the potential to prepare the inertial confinement fusion target with the expected dimension defects, which would advance the application of the AFM tip-based nanomachining approach.

Effect of milling time on microstructure and mechanical properties of Cu-Ni-graphite composites

NASA Astrophysics Data System (ADS)

Wang, Yiran; Gao, Yimin; Li, Yefei; Zhang, Chao; Huang, Xiaoyu; Zhai, Wenyan

2017-09-01

Cu-Ni-graphite composites are intended for application in switch slide baseplate materials. The microstructure of the composites depends strongly on the ball milling time, and a suitable time can significantly improve the properties of the Cu-Ni-graphite composites. In this study, a two-step milling method was employed. The morphology evolution and microstructural features of the powder was characterized at different milling times. Afterwards, the Cu-Ni-graphite composites were prepared in the process of cold pressing, sintering, re-pressing and re-sintering as a function of the different milling times. Finally, both the microstructure and mechanical properties of the Cu-Ni-graphite composites are discussed. The results show that no new phase was generated during the milling process. The morphology evolution of the mixture of Cu/Ni powder changed from spherical-like to cubic-like, plate-like and flake-like with an increasing milling time. The microstructure of the composites consisted of α-phase and graphite. The boundary area and quantity of pores changed as the milling time increased. The relative density, hardness and flexural strength reached maximum values at 15 h of milling time.

Colorimetric protein determination in microalgae (Chlorophyta): association of milling and SDS treatment for total protein extraction.

PubMed

Mota, Maria Fernanda S; Souza, Marcella F; Bon, Elba P S; Rodrigues, Marcoaurelio A; Freitas, Suely Pereira

2018-05-24

The use of colorimetric methods for protein quantification in microalgae is hindered by their elevated amounts of membrane-embedded intracellular proteins. In this work, the protein content of three species of microalgae was determined by the Lowry method after the cells were dried, ball-milled, and treated with the detergent sodium dodecyl sulfate (SDS). Results demonstrated that the association of milling and SDS treatment resulted in a 3- to 7-fold increase in protein quantification. Milling promoted microalgal disaggregation and cell wall disruption enabling access of the SDS detergent to the microalgal intracellular membrane proteins and their efficient solubilization and quantification. © 2018 Phycological Society of America.

Ball mounting fixture for a roundness gage

DOEpatents

Gauler, Allen L.; Pasieka, Donald F.

1983-01-01

A ball mounting fixture for a roundness gage is disclosed. The fixture includes a pair of chuck assemblies oriented substantially transversely with respect to one another and mounted on a common base. Each chuck assembly preferably includes a rotary stage and a wobble plate affixed thereto. A ball chuck affixed to each wobble plate is operable to selectively support a ball to be measured for roundness, with the wobble plate permitting the ball chuck to be tilted to center the ball on the axis of rotation of the rotary stage. In a preferred embodiment, each chuck assembly includes a vacuum chuck operable to selectively support the ball to be measured for roundness. The mounting fixture enables a series of roundness measurements to be taken with a conventional rotating gagehead roundness instrument, which measurements can be utilized to determine the sphericity of the ball.

Ball clay

USGS Publications Warehouse

Virta, R.L.

2013-01-01

Four companies — H.C. Spinks Clay Co., Inc., Imerys, Old Hickory Clay Co. and Unimin Corp. — mined ball clay in five U.S. states in 2012. Production, on the basis of preliminary data, was 900 kt (992,000 st), with an estimated value of $42.3 million. This was a slight increase in tonnage from 886 kt (977,000 st), with a value of $40.9 million in 2011. Tennessee was the leading ball clay producing state, with 63 percent of domestic production, followed by Texas, Mississippi, Kentucky and Indiana. Reported ball clay production from Indiana probably was fire clay rather than ball clay. About 69 percent of total ball clay production was airfloat, 20 percent was crude and 11 percent was water-slurried.

Ball valve extractor

DOEpatents

Herndon, Charles; Brown, Roger A.

2002-01-01

An apparatus and process for removing a ball valve is provided. The ball valve removal tool provides a handle sliding along the length of a shaft. One end of the shaft is secured within an interior cavity of a ball valve while the opposite end of the shaft defines a stop member. By providing a manual sliding force to the handle, the handle impacts the stop member and transmits the force to the ball valve. The direction of the force is along the shaft of the removal tool and disengages the ball valve from the ball valve housing.

Properties of mechanically alloyed Mg-Ni-Ti ternary hydrogen storage alloys for Ni-MH batteries

NASA Astrophysics Data System (ADS)

Ruggeri, Stéphane; Roué, Lionel; Huot, Jacques; Schulz, Robert; Aymard, Luc; Tarascon, Jean-Marie

MgNiTi x, Mg 1- xTi xNi and MgNi 1- xTi x (with x varying from 0 to 0.5) alloys have been prepared by high energy ball milling and tested as hydrogen storage electrodes. The initial discharge capacities of the Mg-Ni-Ti ternary alloys are inferior to the MgNi electrode capacity. However, an exception is observed with MgNi 0.95Ti 0.05, which has an initial discharge capacity of 575 mAh/g compared to 522 mAh/g for the MgNi electrode. The Mg-Ni-Ti ternary alloys show improved cycle life compared to Mg-Ni binary alloys with the same Mg/Ni atomic ratio. The best cycle life is observed with Mg 0.5Ti 0.5Ni electrode which retains 75% of initial capacity after 10 cycles in comparison to 39% for MgNi electrodes, in addition to improved high-rate dischargeability (HRD). According to the XPS analysis, the cycle life improvement of the Mg 0.5Ti 0.5Ni electrode can be related to the formation of TiO 2 which limits Mg(OH) 2 formation. The anodic polarization curve of Mg 0.5Ti 0.5Ni electrode shows that the current related to the active/passive transition is much less important and that the passive region is more extended than for the MgNi electrode but the corrosion of the electrode is still significant. This suggests that the cycle life improvement would be also associated with a decrease of the particle pulverization upon cycling.

Wear resistance of CuZr-based amorphous-forming alloys against bearing steel in 3.5% NaCl solution

NASA Astrophysics Data System (ADS)

Ji, Xiulin; Wang, Hui; Bao, Yayun; Zheng, Dingcong