Experimental Study in Taguchi Method on Surface Quality Predication of HSM

NASA Astrophysics Data System (ADS)

Ji, Yan; Li, Yueen

2018-05-01

Based on the study of ball milling mechanism and machining surface formation mechanism, the formation of high speed ball-end milling surface is a time-varying and cumulative Thermos-mechanical coupling process. The nature of this problem is that the uneven stress field and temperature field affect the machined surface Process, the performance of the processing parameters in the processing interaction in the elastic-plastic materials produced by the elastic recovery and plastic deformation. The surface quality of machining surface is characterized by multivariable nonlinear system. It is still an indispensable and effective method to study the surface quality of high speed ball milling by experiments.

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.

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.

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 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 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

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.

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.

Synthesis of Nano-Crystalline Gamma-TiAl Materials

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Vasquez, Peter

2003-01-01

One of the principal problems with nano-crystalline materials is producing them in quantities and sizes large enough for valid mechanical property evaluation. The purpose of this study was to explore an innovative method for producing nano-crystalline gamma-TiAl bulk materials using high energy ball milling and brief secondary processes. Nano-crystalline powder feedstock was produced using a Fritsch P4(TM) vario-planetary ball mill recently installed at NASA-LaRC. The high energy ball milling process employed tungsten carbide tooling (vials and balls) and no process control agents to minimize contamination. In a collaborative effort, two approaches were investigated, namely mechanical alloying of elemental powders and attrition milling of pre-alloyed powders. The objective was to subsequently use RF plasma spray deposition and short cycle vacuum hot pressing in order to effect consolidation while retaining nano-crystalline structure in bulk material. Results and discussion of the work performed to date are presented.

Effect of processing methods on the mechanical properties of natural rubber filled with stearic acid modified soy protein particles

USDA-ARS?s Scientific Manuscript database

Natural rubber was reinforced with stearic acid modified soy protein particles prepared with a microfluidizing and ball milling process. Longer ball milling time tends to increase tensile strength of the rubber composites. Elastic modulus of the composites increased with the increasing filler concen...

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

Enhanced Magnetic Properties of Nd15Fe77B8 Alloy Powders Produced by Melt-Spinning Technique

NASA Astrophysics Data System (ADS)

Öztürk, Sultan; İcin, Kürşat; Öztürk, Bülent; Topal, Uğur; Odabaşı, Hülya Kaftelen; Göbülük, Metin; Cora, Ömer Necati

2017-10-01

Rapidly solidified Nd15Fe77B8 alloy powders were produced by means of melt-spinning method in high-vacuum atmosphere to achieve improved magnetic and thermal properties. To this goal, a vacuum milling apparatus was designed and constructed to ball-mill the melt-spun powders in a surfactant active atmosphere. Various milling times were experimented to reveal the effect of the milling time on the mean particle size and other size-dependent properties such as magnetism and Curie temperature. Grain structure, cooling rate, and phase structure of the produced powders were also investigated. The Curie points shifted to higher temperatures from the ingot condition to surfactant active ball-milling and the values for Nd15Fe77B8 ingot alloy, melt-spun powders, and surfactant active ball-milled powders were 552 K, 595 K, and 604 K (279 °C, 322 °C, and 331 °C), respectively. It was noted that the surfactant active ball-milling process improved the magnetic and thermal properties of melt-spun Nd15Fe77B8 alloy powders. Compared to relevant literature, the coercivity of powders increased significantly with increasing milling time and decreasing in powder size. The coercivity value as high as 3427 kA m-1 was obtained.

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 SGS modeling enables substantial acceleration of the computing process. There is a visible reduction of the Ra parameter value for milled and burnished surfaces as the burnishing force rises. The tests determined an optimal burnishing force at a level of 500 N (lowest Ra = 0.24 μm). Further increase in the value of burnishing force turned out not to affect the surface roughness, which is consistent with the results obtained from experimental studies.

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%.

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

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

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.

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.

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.

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.

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)

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.

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.

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.

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

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.

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.

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

Size and morphology controlled NiSe nanoparticles as efficient catalyst for the reduction reactions

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

Subbarao, Udumula; Marakatti, Vijaykumar S.; Amshumali, Mungalimane K.

Facile and efficient ball milling and polyol methods were employed for the synthesis of nickel selenide (NiSe) nanoparticle. The particle size of the NiSe nanoparticle has been controlled mechanically by varying the ball size in the milling process. The role of the surfactants in the formation of various morphologies was studied. The compounds were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray energy dispersive spectroscopy (EDS). The efficiency of the NiSe nanoparticle as a catalyst was tested for the reduction of para-nitroaniline (PNA) to para-phenyldiamine (PPD) and para-nitrophenol (PNP) to para-aminophenol (PAP)more » using NaBH{sub 4} as the reducing agent. Particle size, morphology and the presence of surfactant played a crucial role in the reduction process. - Graphical abstract: NiSe nanoparticles in different size and morphology were synthesized using facile ball milling and polyol methods. Particle size, morphology and the presence of surfactant in these materials played a crucial role in the hydrogenation of PNA and PNP. - Highlights: • NiSe nanoparticles synthesized using ball milling and solution phase methods. • NiSe nanoparticle is an efficient catalyst for the reduction of PNA and PNP. • NiSe is found to be better than the best reported noble metal catalysts.« less

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

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

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

Kou, Hongchao; Hou, Xiaojiang; Zhang, Tiebang, E-mail: tiebangzhang@nwpu.edu.cn

2013-06-15

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

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

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

Taghvaei, Amir Hossein, E-mail: Amirtaghvaei@gmail.com; Department of Materials Science and Engineering, Shiraz University of Technology, Shiraz; Stoica, Mihai

2014-06-01

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

Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering

PubMed Central

Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

2015-01-01

The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 oC, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase. PMID:26369360

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

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%.

Effect of ball milling on the physicochemical properties of atorvastatin calcium sesquihydrate: the dissolution kinetic behaviours of milled amorphous solids.

PubMed

Kobayashi, Makiko; Hattori, Yusuke; Sasaki, Tetsuo; Otsuka, Makoto

2017-01-01

The purposes of this study were to clarify the amorphization by ball milling of atorvastatin calcium sesquihydrate (AT) and to analyse the change in dissolution kinetics. The amorphous AT was prepared from crystal AT by ball milling and analysed in terms of the changes of its physicochemical properties by powder X-ray diffraction analysis (XRD), thermal analysis and infrared spectroscopy (IR). Moreover, to evaluate the usefulness of the amorphous form for pharmaceutical development, intrinsic solubility of the ground product was evaluated using a dissolution kinetic method. The XRD results indicated that crystalline AT was transformed into amorphous solids by more than 30-min milling. The thermal analysis result suggested that chemical potential of the ground AT are changed significantly by milling. The IR spectra of the AT showed the band shift from the amide group at 3406 cm -1 with an intermolecular hydrogen bond to a free amide group at 3365 cm -1 by milling. The dissolution of amorphous AT follows a dissolution kinetic model involving phase transformation. The initial dissolution rate of the ground product increased with the increase in milling time to reflect the increase in the intrinsic solubility based on the amorphous state. © 2016 Royal Pharmaceutical Society.

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

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.

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.

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

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...

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.

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.

Hot pressing titanium metal matrix composites reinforced with graphene nanoplatelets through an in-situ reactive method

NASA Astrophysics Data System (ADS)

Mu, X. N.; Zhang, H. M.; Cai, H. N.; Fan, Q. B.; Wu, Y.; Fu, Z. J.; Wang, Q. X.

2017-05-01

This study proposed an in-situ reactive method that uses graphene as a reinforcement to fabricate titanium metal matrix composites (TiMMCs) through powder metallurgy processing route. The volume fraction of graphene nanoplatelets was 1.8%vol, and the pure titanium was used as a matrix. The Archimedes density, hardness, microstructure and mechanical properties of specimens were compared under different ball milling times (20 min and 2.5 h) and hot pressing temperatures (900°C, 1150°C, and 1300°C,). The ultimate tensile strength of 630 MPa, which demonstrated a 27.3% increase compared with pure Ti, was achieved under a ball milling time of 20 min. Elongation increased with increasing temperature. When the ball milling time and hot pressing temperature were increased to 2.5 h and 1300 °C, respectively, the ultimate tensile strength of the composites reached 750 MPa, showing an increase of 51.5% compared with pure Ti.

Novel technology to prepare oral formulations for preclinical safety studies.

PubMed

Niwa, Toshiyuki; Hashimoto, Naofumi

2008-02-28

A novel method to prepare oral formulations, normally suspended dosage form, for preclinical safety studies in animals has been developed using a rotation/revolution mixer. Small hard balls made of zirconia were added to the mixing process to evaluate effectiveness in making a high quality suspension. The driving with balls loaded in the cylindrical container (vessel) of the mixer was quite efficient in dispersing and milling the particles of the active pharmaceutical ingredient (API) in an aqueous medium. The API powder and a small amount of oral aqueous medium (vehicle) were successfully mixed by the spinning motion of the balls in the vessel as though the paste-like suspension was kneaded with a mortar and pestle. It was found that the milled suspension with the mean size of 10-20microm could be prepared, in addition finer milling of less than 10microm could be achieved by selecting the material of vessel. Optimum driving conditions including mixing time, size and quantity of balls, and the standard operational procedure was established using compounds varying in physicochemical properties. The particle size and quantitative analysis by HPLC showed that the resultant suspension was well-milled and highly homogeneous with the nearly intended concentration of API. The proposed method established by this experiment could be applied to the actual safety studies in the real preparation scale of oral suspension.

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.

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.

Systematic comparison of mechanical and thermal sludge disintegration technologies.

PubMed

Wett, B; Phothilangka, P; Eladawy, A

2010-06-01

This study presents a systematic comparison and evaluation of sewage sludge pre-treatment by mechanical and thermal techniques. Waste activated sludge (WAS) was pre-treated by separate full scale Thermo-Pressure-Hydrolysis (TDH) and ball milling facilities. Then the sludge was processed in pilot-scale digestion experiments. The results indicated that a significant increase in soluble organic matter could be achieved. TDH and ball milling pre-treatment could offer a feasible treatment method to efficiently disintegrate sludge and enhance biogas yield of digestion. The TDH increased biogas production by ca. 75% whereas ball milling allowed for an approximately 41% increase. The mechanisms of pre-treatment were investigated by numerical modeling based on Anaerobic Digestion Model No. 1 (ADM1) in the MatLab/SIMBA environment. TDH process induced advanced COD-solubilisation (COD(soluble)/COD(total)=43%) and specifically complete destruction of cell mass which is hardly degradable in conventional digestion. While the ball mill technique achieved a lower solubilisation rate (COD(soluble)/COD(total)=28%) and only a partial destruction of microbial decay products. From a whole-plant prospective relevant release of ammonia and formation of soluble inerts have been observed especially from thermal hydrolysis. Copyright 2009 Elsevier Ltd. All rights reserved.

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.

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.

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.

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.

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

PubMed Central

Manukyan, Khachatur V.; Shuck, Christopher E.; Rogachev, Alexander S.; Mukasyan, Alexander S.

2015-01-01

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the balls. Among other applications, it is a versatile technique that allows for effective preparation of gasless reactive nanostructured materials with high energy density per volume (Ni+Al, Ta+C, Ti+C). The structural transformations of reactive media, which take place during HEBM, define the reaction mechanism in the produced energetic composites. Varying the processing conditions permits fine tuning of the milling-induced microstructures of the fabricated composite particles. In turn, the reactivity, i.e., self-ignition temperature, ignition delay time, as well as reaction kinetics, of high energy density materials depends on its microstructure. Analysis of the milling-induced microstructures suggests that the formation of fresh oxygen-free intimate high surface area contacts between the reagents is responsible for the enhancement of their reactivity. This manifests itself in a reduction of ignition temperature and delay time, an increased rate of chemical reaction, and an overall decrease of the effective activation energy of the reaction. The protocol provides a detailed description for the preparation of reactive nanocomposites with tailored microstructure using short-term HEBM method. It also describes a high-speed thermal imaging technique to determine the ignition/combustion characteristics of the energetic materials. The protocol can be adapted to preparation and characterization of a variety of nanostructured energetic composites. PMID:25868065

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

Investigation of enzyme formulation on pretreated switchgrass.

PubMed

Falls, Matthew; Shi, Jian; Ebrik, Mirvat A; Redmond, Tim; Yang, Bin; Wyman, Charles E; Garlock, Rebecca; Balan, Venkatesh; Dale, Bruce E; Pallapolu, V Ramesh; Lee, Y Y; Kim, Youngmi; Mosier, Nathan S; Ladisch, Michael R; Hames, Bonnie; Thomas, Steve; Donohoe, Bryon S; Vinzant, Todd B; Elander, Richard T; Warner, Ryan E; Sierra-Ramirez, Rocio; Holtzapple, Mark T

2011-12-01

This work studied the benefits of adding different enzyme cocktails (cellulase, xylanase, β-glucosidase) to pretreated switchgrass. Pretreatment methods included ammonia fiber expansion (AFEX), dilute-acid (DA), liquid hot water (LHW), lime, lime+ball-milling, soaking in aqueous ammonia (SAA), and sulfur dioxide (SO(2)). The compositions of the pretreated materials were analyzed and showed a strong correlation between initial xylan composition and the benefits of xylanase addition. Adding xylanase dramatically improved xylan yields for SAA (+8.4%) and AFEX (+6.3%), and showed negligible improvement (0-2%) for the pretreatments with low xylan content (dilute-acid, SO(2)). Xylanase addition also improved overall yields with lime+ball-milling and SO(2) achieving the highest overall yields from pretreated biomass (98.3% and 93.2%, respectively). Lime+ball-milling obtained an enzymatic yield of 92.3kg of sugar digested/kg of protein loaded. Copyright © 2011 Elsevier Ltd. All rights reserved.

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.

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.

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.

Microstructural Evolution of Dy2O3-TiO2 Powder Mixtures during Ball Milling and Post-Milled Annealing

PubMed Central

Huang, Jinhua; Ran, Guang; Lin, Jianxin; Shen, Qiang; Lei, Penghui; Wang, Xina; Li, Ning

2016-01-01

The microstructural evolution of Dy2O3-TiO2 powder mixtures during ball milling and post-milled annealing was investigated using XRD, SEM, TEM, and DSC. At high ball-milling rotation speeds, the mixtures were fined, homogenized, nanocrystallized, and later completely amorphized, and the transformation of Dy2O3 from the cubic to the monoclinic crystal structure was observed. The amorphous transformation resulted from monoclinic Dy2O3, not from cubic Dy2O3. However, at low ball-milling rotation speeds, the mixtures were only fined and homogenized. An intermediate phase with a similar crystal structure to that of cubic Dy2TiO5 was detected in the amorphous mixtures annealed from 800 to 1000 °C, which was a metastable phase that transformed to orthorhombic Dy2TiO5 when the annealing temperature was above 1050 °C. However, at the same annealing temperatures, pyrochlore Dy2Ti2O7 initially formed and subsequently reacted with the remaining Dy2O3 to form orthorhombic Dy2TiO5 in the homogenous mixtures. The evolutionary mechanism of powder mixtures during ball milling and subsequent annealing was analyzed. PMID:28772375

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.

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.

Crystalline maricite NaFePO4 as a positive electrode material for sodium secondary batteries operating at intermediate temperature

NASA Astrophysics Data System (ADS)

Hwang, Jinkwang; Matsumoto, Kazuhiko; Orikasa, Yuki; Katayama, Misaki; Inada, Yasuhiro; Nohira, Toshiyuki; Hagiwara, Rika

2018-02-01

Maricite NaFePO4 (m-NaFePO4) was investigated as a positive electrode material for intermediate-temperature operation of sodium secondary batteries using ionic liquid electrolytes. Powdered m-NaFePO4 was prepared by a conventional solid-state method at 873 K and subsequently fabricated in two different conditions; one is ball-milled in acetone and the other is re-calcined at 873 K after the ball-milling. Electrochemical properties of the electrodes prepared with the as-synthesized m-NaFePO4, the ball-milled m-NaFePO4, and the re-calcined m-NaFePO4 were investigated in Na[FSA]-[C2C1im][FSA] (C2C1im+ = 1-ethyl-3-methylimidazolium, FSA- = bis(fluorosulfonyl)amide) ionic liquid electrolytes at 298 K and 363 K to assess the effects of temperature and particle size on their electrochemical properties. A reversible charge-discharge capacity of 107 mAh g-1 was achieved with a coulombic efficiency >98% from the 2nd cycle using the ball-milled m-NaFePO4 electrode at a C-rate of 0.1 C and 363 K. Electrochemical impedance spectroscopy using m-NaFePO4/m-NaFePO4 symmetric cells indicated that inactive m-NaFePO4 becomes an active material through ball-milling treatment and elevation of operating temperature. X-ray diffraction analysis of crystalline m-NaFePO4 confirmed the lattice contraction and expansion upon charging and discharging, respectively. These results indicate that the desodiation-sodiation process in m-NaFePO4 is reversible in the intermediate-temperature range.

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.

Effect of heat treatment and ball milling on MnBi magnetic materials

NASA Astrophysics Data System (ADS)

Li, Chunhong; Guo, Donglin; Shao, Bin; Li, Kejian; Li, Bingbing; Chen, Dengming

2018-01-01

MnBi alloy was prepared using arc melting, and was then heated at various temperatures and times. The alloy was ball milled for various lengths of time, following a heat treatment at 573 K for 20 h. The effects of the heat treatment and the ball milling on the magnetic performances of the material were investigated by analyzing the phases, the particle sizes, and the grain sizes. Results showed that the mass percentage of the LTP MnBi phase increased as the heat treatment time increased. The mass percentage initially increased and then decreased as the heat treatment temperature increased. The saturation magnetization increased quickly as the mass percentage of the LTP MnBi increased following the heat treatment. The value rose as high as 71.39 emu g-1 at 573 K for 30 h. The magnetization decreased, due to the decomposition of MnBi phases after ball milling. The coercivity increased simultaneously, due to the grain refinement, the presence of stresses, defects, and an amorphous phase. This value was improved from 0.09 to 14.65 KOe after ball milling for 24 h.

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.

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

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

Mechanically Induced Graphite-Nanodiamonds-Phase Transformations During High-Energy Ball Milling

NASA Astrophysics Data System (ADS)

El-Eskandarany, M. Sherif

2017-05-01

Due to their unusual mechanical, chemical, physical, optical, and biological properties, nearly spherical-like nanodiamonds have received much attention as desirable advanced nanomaterials for use in a wide spectrum of applications. Although, nanodiamonds can be successfully synthesized by several approaches, applications of high temperature and/or high pressure may restrict the real applications of such strategic nanomaterials. Distinct from the current preparation approaches used for nanodiamonds preparation, here we show a new process for preparing ultrafine nanodiamonds (3-5 nm) embedded in a homogeneous amorphous-carbon matrix. Our process started from high-energy ball milling of commercial graphite powders at ambient temperature under normal atmospheric helium gas pressure. The results have demonstrated graphite-single wall carbon nanotubes-amorphous-carbon-nanodiamonds phase transformations carried out through three subsequent stages of ball milling. Based on XRD and RAMAN analyses, the percentage of nanodiamond phase + C60 (crystalline phase) produced by ball milling was approximately 81%, while the amorphous phase amount was 19%. The pressure generated on the powder together the with temperature increase upon the ball-powder-ball collision is responsible for the phase transformations occurring in graphite powders.

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

Processing study of high temperature superconducting Y-Ba-Cu-O ceramics

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

Safari, A.; Wachtman, J.B. Jr.; Ward, C.

Processing of the YBa{sub 2}Cu{sub 3}O{sub 6+x} superconducting phase by employing different precursor powder preparation techniques (ball milling, attrition milling) and samples formed by different sintering conditions are discussed. The superconducting phase has been identified by powder x-ray diffraction. The effect of different powder processing and pressing conditions on the structure, density, resistivity and a.c. magnetic susceptibility were studied. Though there is no variation in T{sub c} for all the samples, attrition milled samples show a much lower resistance and less temperature dependence compared to ball milled samples above the superconducting transition temperature up to room temperature. Ball milled samplesmore » were loosely packed with more voids compared to attrition milled samples which are more densely packed with a needle-like structure.« 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

Toward a better understanding of the lignin isolation process from wood.

PubMed

Guerra, Anderson; Filpponen, Ilari; Lucia, Lucian A; Saquing, Carl; Baumberger, Stephanie; Argyropoulos, Dimitris S

2006-08-09

The recently developed protocol for isolating enzymatic mild acidolysis lignins (EMAL) coupled with the novel combination of derivatization followed by reductive cleavage (DFRC) and quantitative (31)P NMR spectroscopy were used to better understand the lignin isolation process from wood. The EMAL protocol is shown to offer access at lignin samples that are more representative of the overall lignin present in milled wood. The combination of DFRC/(31)P NMR provided a detailed picture on the effects of the isolation conditions on the lignin structure. More specifically, we have used vibratory and ball milling as the two methods of wood pulverization and have compared their effects on the lignin structures and molecular weights. Vibratory-milling conditions cause substantial lignin depolymerization. Lignin depolymerization occurs via the cleavage of uncondensed beta-aryl ether linkages, while condensed beta-aryl ethers and dibenzodioxocins were found to be resistant to such mechanical action. Condensation and side chain oxidations were induced mechanochemically under vibratory-milling conditions as evidenced by the increased amounts of condensed phenolic hydroxyl and carboxylic acid groups. Alternatively, the mild mechanical treatment offered by ball milling was found not to affect the isolated lignin macromolecular structure. However, the overall lignin yields were found to be compromised when the mechanical action was less intense, necessitating longer milling times under ball-milling conditions. As compared to other lignin preparations isolated from the same batch of milled wood, the yield of EMAL was about four times greater than the corresponding milled wood lignin (MWL) and about two times greater as compared to cellulolytic enzyme lignin (CEL). Molecular weight distribution analyses also pointed out that the EMAL protocol allows the isolation of lignin fractions that are not accessed by any other lignin isolation procedures.

Mutual solubility of scandium oxide-hematite magnetic nanocomposites: Mössbauer spectroscopy investigation

NASA Astrophysics Data System (ADS)

Allwes, Mark; Mekaoui, Mehdi; Sorescu, Monica

2017-08-01

xSc2O3-(1-x)α-Fe2O3 (x = 0.1, 0.3 and 0.5) nanocomposite systems were successfully synthesized by mechanochemical activation of Sc2O3 and α-Fe2O3 mixtures for 0-12 h of ball milling time. Mössbauer investigations were performed to study the structural and magnetic properties of xSc2O3-(1-x)α-Fe2O3 nanoparticle systems during the mechanochemical activation treatment. The Mössbauer studies showed that the spectrum of the mechanochemically activated composites evolved from a sextet for hematite to sextets and a doublet upon duration of the milling process with scandium oxide. Mutual solubility was achieved at the nanoscopic level only. A comprehensive Mössbauer study was performed by recording the recoilless fraction f as function of the ball milling time using our dual absorber method. The results obtained indicate that prolonged ball milling times favor formation of the Fe:Sc2O3 non-magnetic phase and decrease of the grain sizes for both magnetic and non-magnetic components, leading to a maximum in the recoilless fraction followed by its decay.

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.

Influence of stacking fault energy on defect structures and microhardness of Cu and Cu alloys.

PubMed

Tao, Jing-Mei; Li, Dai; Li, Cai-Ju; Zhu, Xin-Kun

2011-12-01

Nano-structured Cu, Cu-10 wt%Zn and Cu-2 wt%Al with stacking fault energies (SFE) of 78, 35 and 37 mJ/m2, respectively, were preprared through high energy ball milling. X-ray diffraction and Vickers microharness test were used to investigate the microstructure and microhardness of all the samples after ball milling. X-ray diffraction measurements indicate that lower SFEs lead both to decrease in grain size and increase in microstrain, dislocation and twin densities for Cu-10 wt%Zn and Cu-2 wt%Al after 5 h of ball milling. The microhardnesses of Cu-10 wt%Zn and Cu-2 wt%Al reach to nearly the same values of 2.5 GPa after 5 h of ball milling, which is higher than that of Cu of 2.0 GPa. Two factors are considered to contribute to the finer grian size and higher microhardness of Cu-10 wt%Zn and Cu-2 wt%Al: (1) the effect of solid solution strengthening, which result in the interaction of solute atoms with screw dislocations; (2) the introduction of deformation twins during ball milling process by the decreasing of SFE, which results in the grain refinement.

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.

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

Fabrication of novel cryomill for synthesis of high purity metallic nanoparticles

NASA Astrophysics Data System (ADS)

Kumar, Nirmal; Biswas, Krishanu

2015-08-01

The successful preparation of free standing metal nanoparticles with high purity in bulk quantity is the pre-requisite for any potential application. This is possible by using ball milling at cryogenic temperature. However, the most of ball mills available in the market do not allow preparing high purity metal nanoparticles by this route. In addition, it is not possible to carry out in situ measurements of process parameters as well as diagnostic of the process. In the present investigation, we present a detailed study on the fabrication of a cryomill, which is capable of avoiding contaminations in the product. It also provides in situ measurements and diagnostic of the low temperature milling process. Online monitoring of the milling temperature and observation of ball motion are the important aspects in the newly designed mill. The nanoparticles prepared using this fabricated mill have been found to be free standing and also free from contaminations.

Decoupling the Arrhenius equation via mechanochemistry.

PubMed

Andersen, Joel M; Mack, James

2017-08-01

Mechanochemistry continues to reveal new possibilities in chemistry including the opportunity for "greening" reactions. Nevertheless, a clear understanding of the energetic transformations within mechanochemical systems remains elusive. We employed a uniquely modified ball mill and strategically chosen Diels-Alder reactions to evaluate the role of several ball-milling variables. This revealed three different energetic regions that we believe are defining characteristics of most, if not all, mechanochemical reactors. Relative to the locations of a given ball mill's regions, activation energy determines whether a reaction is energetically easy (Region I), challenging (Region II), or unreasonable (Region III) in a given timeframe. It is in Region II, that great sensitivity to mechanochemical conditions such as vial material and oscillation frequency emerge. Our unique modifications granted control of reaction vessel temperature, which in turn allowed control of the locations of Regions I, II, and III for our mill. Taken together, these results suggest envisioning vibratory mills (and likely other mechanochemical methodologies) as molecular-collision facilitating devices that act upon molecules occupying a thermally-derived energy distribution. This unifies ball-milling energetics with solution-reaction energetics via a common tie to the Arrhenius equation, but gives mechanochemistry the unique opportunity to influence either half of the equation. In light of this, we discuss a strategy for translating solvent-based reaction conditions to ball milling conditions. Lastly, we posit that the extra control via frequency factor grants mechanochemistry the potential for greater selectivity than conventional solution reactions.

Formation of budesonide/α-lactose glass solutions by ball-milling

NASA Astrophysics Data System (ADS)

Dudognon, E.; Willart, J. F.; Caron, V.; Capet, F.; Larsson, T.; Descamps, M.

2006-04-01

The possibility to obtain amorphous budesonide stabilised by blending with an excipient characterised by a higher glass transition temperature, namely α-lactose, has been studied. We carried out the mixing of the two compounds at room temperature by ball-milling. The four obtained blends (containing, respectively, 10, 30, 50 and 70% w of budesonide) are X-ray amorphous and exhibit a single glass transition located between the ones of pure milled crystalline compounds. This revealed that the two amorphous phases are miscible whatever the composition and sufficiently mixed to relax as a whole. Ball-milling thus appears as a powerful tool to form amorphous molecular alloys with enhanced stability properties.

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.

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.

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 decreasing amount of SL, whereas in the case of the co-milled formulations, the higher the amount of SL in the glassy solution is, the higher the amount of TD dissolved. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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.

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 materials essentially because of the overall complexity of the oxide structures, of their surfaces, of their defects and of their mechanical behavior.

Mechanical alloying of lanthana-bearing nanostructured ferritic steels

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

Somayeh Paseban; Indrajit Charit; Yaqiao Q. Wu

2013-09-01

A novel nanostructured ferritic steel powder with the nominal composition Fe–14Cr–1Ti–0.3Mo–0.5La2O3 (wt.%) was developed via high energy ball milling. La2O3 was added to this alloy instead of the traditionally used Y2O3. The effects of varying the ball milling parameters, such as milling time, steel ball size and ball to powder ratio, on the mechanical properties and micro structural characteristics of the as-milled powder were investigated. Nanocrystallites of a body-centered cubic ferritic solid solution matrix with a mean size of approximately 20 nm were observed by transmission electron microscopy. Nanoscale characterization of the as-milled powder by local electrode atom probe tomographymore » revealed the formation of Cr–Ti–La–O-enriched nanoclusters during mechanical alloying. The Cr:Ti:La:O ratio is considered “non-stoichiometric”. The average size (radius) of the nanoclusters was about 1 nm, with number density of 3.7 1024 m3. The mechanism for formation of nanoclusters in the as-milled powder is discussed. La2O3 appears to be a promising alternative rare earth oxide for future nanostructured ferritic steels.« 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 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

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.

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.

Minimisation of costs by using disintegration at a full-scale anaerobic digestion plant.

PubMed

Winter, A

2002-01-01

Various half-scale and lab-scale investigations have already shown that the disintegration of excess sludge is a possible pre-treatment to optimise anaerobic digestion. To control these results different methods of disintegration were investigated at a full-scale plant. Two stirred ball mills and a plant for oxidation with ozone were applied. A positive influence of disintegration on the anaerobic biodegradability can be established with application of a stirred ball mill. Biogas production as well as the degree of degradation were increased by about 20%. Laboratory investigations also validate that disintegration increases the polymer demand and leads to a lower solid content after dewatering. A higher pollution level of process water after dewatering even with ammonia and COD corroborates the results of the anaerobic degradation. Capital costs for the stirred ball mill, costs for energy, manpower and maintenance can be covered if the specific costs for disposal are high. If the development of costs in future and the current discussion about sludge disposal are taken into account sewage sludge disintegration can be a suitable technique to minimise costs at waste water treatment plants.

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.

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries

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

Wang , Jing; Bao, Wurigumula; Ma, Lu

2015-11-09

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide–nickel–graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx/Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stickmore » well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx/Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials.« less

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries.

PubMed

Wang, Jing; Bao, Wurigumula; Ma, Lu; Tan, Guoqiang; Su, Yuefeng; Chen, Shi; Wu, Feng; Lu, Jun; Amine, Khalil

2015-12-07

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide-nickel-graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx /Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stick well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx /Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

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.

A Holistic Multi Evidence Approach to Study the Fragmentation Behaviour of Crystalline Mannitol

PubMed Central

Koner, Jasdip S.; Rajabi-Siahboomi, Ali; Bowen, James; Perrie, Yvonne; Kirby, Daniel; Mohammed, Afzal R.

2015-01-01

Mannitol is an essential excipient employed in orally disintegrating tablets due to its high palatability. However its fundamental disadvantage is its fragmentation during direct compression, producing mechanically weak tablets. The primary aim of this study was to assess the fracture behaviour of crystalline mannitol in relation to the energy input during direct compression, utilising ball milling as the method of energy input, whilst assessing tablet characteristics of post-milled powders. Results indicated that crystalline mannitol fractured at the hydrophilic (011) plane, as observed through SEM, alongside a reduction in dispersive surface energy. Disintegration times of post-milled tablets were reduced due to the exposure of the hydrophilic plane, whilst more robust tablets were produced. This was shown through higher tablet hardness and increased plastic deformation profiles of the post-milled powders, as observed with a lower yield pressure through an out-of-die Heckel analysis. Evaluation of crystal state using x-ray diffraction/differential scanning calorimetry showed that mannitol predominantly retained the β-polymorph; however x-ray diffraction provided a novel method to calculate energy input into the powders during ball milling. It can be concluded that particle size reduction is a pragmatic strategy to overcome the current limitation of mannitol fragmentation and provide improvements in tablet properties. PMID:26553127

A Holistic Multi Evidence Approach to Study the Fragmentation Behaviour of Crystalline Mannitol

NASA Astrophysics Data System (ADS)

Koner, Jasdip S.; Rajabi-Siahboomi, Ali; Bowen, James; Perrie, Yvonne; Kirby, Daniel; Mohammed, Afzal R.

2015-11-01

Mannitol is an essential excipient employed in orally disintegrating tablets due to its high palatability. However its fundamental disadvantage is its fragmentation during direct compression, producing mechanically weak tablets. The primary aim of this study was to assess the fracture behaviour of crystalline mannitol in relation to the energy input during direct compression, utilising ball milling as the method of energy input, whilst assessing tablet characteristics of post-milled powders. Results indicated that crystalline mannitol fractured at the hydrophilic (011) plane, as observed through SEM, alongside a reduction in dispersive surface energy. Disintegration times of post-milled tablets were reduced due to the exposure of the hydrophilic plane, whilst more robust tablets were produced. This was shown through higher tablet hardness and increased plastic deformation profiles of the post-milled powders, as observed with a lower yield pressure through an out-of-die Heckel analysis. Evaluation of crystal state using x-ray diffraction/differential scanning calorimetry showed that mannitol predominantly retained the β-polymorph however x-ray diffraction provided a novel method to calculate energy input into the powders during ball milling. It can be concluded that particle size reduction is a pragmatic strategy to overcome the current limitation of mannitol fragmentation and provide improvements in tablet properties.

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

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.

Phase transformations in the hematite-metal system during mechanical alloying

NASA Astrophysics Data System (ADS)

Kozlov, K. A.; Shabashov, V. A.; Litvinov, A. V.; Sagaradze, V. V.

2009-04-01

Mössbauer spectroscopy and X-ray diffraction are used to show that the phase transformations in hematite α-Fe2O3-metal ( M = Fe, Ni, Ti, Zr) powder mixtures induced by severe cold plastic deformation in ball mills occur via the formation of M-Fe-O solid solutions, redox reactions with the reduction of metallic iron, and the formation of secondary M x O y oxides and M x Fe y intermetallics. Mechanical activation in a ball mill is compared to that under high-pressure shear in Bridgman anvils. The transformations that take place in a ball mill are found to have several stages and to be accelerated.

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

Novel high pressure hexagonal OsB2 by mechanochemistry

NASA Astrophysics Data System (ADS)

Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

2014-07-01

Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

Effect of microfluidized and stearic acid modified soy protein in natural rubber

USDA-ARS?s Scientific Manuscript database

Microfluidized and stearic acid modified soy protein aggregates were used to reinforced natural rubber. The size of soy protein particles was reduced with a microfluidizing and ball milling process. Filler size reduction with longer ball milling time tends to increase tensile strength of the rubber ...

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.

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.

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

Rounaghi, S.A., E-mail: s.a.rounaghi@gmail.com; Kiani Rashid, A.R.; Eshghi, H., E-mail: heshghi@ferdowsi.um.ac.ir

Decomposition of melamine was studied by solid state reaction of melamine and aluminum powders during high energy ball-milling. The milling procedure performed for both pure melamine and melamine/Al mixed powders as the starting materials for various times up to 48 h under ambient atmosphere. The products were characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results revealed that Al causes melamine deammoniation at the first stages of milling and further milling process leads to the s-triazine ring degradation while nano-crystallite hexagonal aluminum nitride (h-AlN) was the main solid product. Comparison to milling process, the possibility ofmore » the reaction of melamine with Al was also investigated by thermal treatment method using differential scanning calorimeter (DSC) and thermo gravimetric analyzer (TGA). Melamine decomposition occurred by thermal treatment in the range of 270-370 Degree-Sign C, but no reaction between melamine and aluminum was observed. - Graphical Abstract: Mechanochemical reaction of melamine with Al resulted in the formation of nanocrystalline AlN after 7 h milling time Highlights: Black-Right-Pointing-Pointer High energy ball milling of melamine and aluminum results decomposition of melamine with elimination of ammonia. Black-Right-Pointing-Pointer Nano-crystalline AlN was synthesized by the mechanochemical route. Black-Right-Pointing-Pointer Milling process has no conspicuous effect on pure melamine degradation. Black-Right-Pointing-Pointer No reaction takes place by heating melamine and aluminum powder mixture in argon.« less

Mechanochemical Ring-Opening Polymerization of Lactide: Liquid-Assisted Grinding for the Green Synthesis of Poly(lactic acid) with High Molecular Weight.

PubMed

Ohn, Nuri; Shin, Jihoon; Kim, Sung Sik; Kim, Jeung Gon

2017-09-22

Mechanochemical polymerization of lactide is carried out by using ball milling. Mechanical energy from collisions between the balls and the vessel efficiently promotes an organic-base-mediated metal- and solvent-free solid-state polymerization. Investigation of the parameters of the ball-milling synthesis revealed that the degree of lactide ring-opening polymerization could be modulated by the ball-milling time, vibration frequency, mass of the ball media, and liquid-assisted grinding. Liquid-assisted grinding was found to be an especially important factor for achieving a high degree of mechanochemical polymerization. Although polymer-chain scission from the strong collision energy prevented mechanical-force-driven high-molecular-weight polymer synthesis, the addition of only a small amount of liquid enabled sufficient energy dissipation and poly(lactic acid) was thereby obtained with a molecular weight of over 1×10 5  g mol -1 . © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fabrication of Aluminum Foams with Small Pore Size by Melt Foaming Method

NASA Astrophysics Data System (ADS)

Cheng, Ying; Li, Yanxiang; Chen, Xiang; Shi, Tong; Liu, Zhiyong; Wang, Ningzhen

2017-04-01

This article introduces an improvement to the fabrication of aluminum foams with small pore size by melt foaming method. Before added to the melt, the foaming agent (titanium hydride) was pretreated in two steps. It firstly went through the traditional pre-oxidation treatment, which delayed the decomposition of titanium hydride and made sure the dispersion stage was controllable. Then such pre-oxidized titanium hydride powder was mixed with copper powder in a planetary ball mill. This treatment can not only increase the number of foaming agent particles and make them easier to disperse in the melt, which helps to increase the number of pores, but also reduce the amount of hydrogen released in the foaming stage. Therefore, the pore size could be decreased. Using such a ball-milled foaming agent in melt foaming method, aluminum foams with small pore size (average size of 1.6 mm) were successfully fabricated.

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 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.

Fracture Surface Morphology and Impact Strength of Cellulose/PLA Composites.

PubMed

Gao, Honghong; Qiang, Tao

2017-06-07

Polylactide (PLA)-based composite materials reinforced with ball-milled celluloses were manufactured by extrusion blending followed by injection molding. Their surface morphology from impact fracture were imaged with scanning electron microscopy (SEM) and investigated by calculating their fractal dimensions. Then, linear regression was used to explore the relationship between fractal dimension and impact strength of the resultant cellulose/PLA composite materials. The results show that filling the ball-milled celluloses into PLA can improve the impact toughness of PLA by a minimum of 38%. It was demonstrated that the fracture pattern of the cellulose/PLA composite materials is different from that of pristine PLA. For the resultant composite materials, the fractal dimension of the impact fractured surfaces increased with increasing filling content and decreasing particle size of the ball-milled cellulose particles. There were highly positive correlations between fractal dimension of the fractured surfaces and impact strength of the cellulose/PLA composites. However, the linearity between fractal dimension and impact strength were different for the different methods, due to their different R-squared values. The approach presented in this work will help to understand the structure-property relationships of composite materials from a new perspective.

Fracture Surface Morphology and Impact Strength of Cellulose/PLA Composites

PubMed Central

Gao, Honghong; Qiang, Tao

2017-01-01

Polylactide (PLA)-based composite materials reinforced with ball-milled celluloses were manufactured by extrusion blending followed by injection molding. Their surface morphology from impact fracture were imaged with scanning electron microscopy (SEM) and investigated by calculating their fractal dimensions. Then, linear regression was used to explore the relationship between fractal dimension and impact strength of the resultant cellulose/PLA composite materials. The results show that filling the ball-milled celluloses into PLA can improve the impact toughness of PLA by a minimum of 38%. It was demonstrated that the fracture pattern of the cellulose/PLA composite materials is different from that of pristine PLA. For the resultant composite materials, the fractal dimension of the impact fractured surfaces increased with increasing filling content and decreasing particle size of the ball-milled cellulose particles. There were highly positive correlations between fractal dimension of the fractured surfaces and impact strength of the cellulose/PLA composites. However, the linearity between fractal dimension and impact strength were different for the different methods, due to their different R-squared values. The approach presented in this work will help to understand the structure–property relationships of composite materials from a new perspective. PMID:28772983

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.

Synthesis and characterization of NaCo(1-x)MnxO2 solid electrolyte using sol-gel method: the effect of milling speed variations

NASA Astrophysics Data System (ADS)

Suyati, L.; Widyayanti, O. A.; Qushoyyi, M.; Darmawan, A.; Nuryanto, R.

2018-04-01

Battery is a device that converts chemical energy into electrical energy through electrochemical process. Further research on the synthesis of cathode of Na-ion battery that has good conductivity to maximize the battery performance needs to be conducted. One of the production steps of the NaCo(1-x)NaCo cathode synthesis in the Na-Ion battery was a ball-milling process, in which by the ball-milling process, the crystal size of NaCo(1-x)MnxO2 cathode can be minimized. The purpose of this study was to determine the effect of variation of ball-milling speed to the characteristics of resulting product including the oxide types composing NaCo(1-x)MnxO2 cathode, surface morphology, and conductivity. The main ingredients used were sodium acetate, manganese acetate, cobalt acetate with molar ratio of 0.7: 0.66: 0.22, respectively and citric acid as chelating agent with the M/CA ratio of 1: 1. The variations of milling speed were 0, 300, 400, 500, 600 and 700 rpm. Characterization of the product was conducted using XRD, SEM-EDS, and conductivity meter (LCR-meter). The result showed that a solid electrolyte of NaCo(1-x)MnxO2 consisting of NaMnO2, NaO2, CoO, Co2O3, MnO2 components was successfully synthesized. The observation on the milling speed at 400 rpm showed that the solid electrolyte produced had the highest conductivity i.e. 4.08 x 10-6 Scm-1 with a homogeneous surface morphology and had a spinel formula NaCo0,65Mn0,35O2.

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.

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.

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.

Formulation of a dry powder influenza vaccine for nasal delivery.

PubMed

Garmise, Robert J; Mar, Kevin; Crowder, Timothy M; Hwang, C Robin; Ferriter, Matthew; Huang, Juan; Mikszta, John A; Sullivan, Vincent J; Hickey, Anthony J

2006-03-10

The purpose of this research was to prepare a dry powder vaccine formulation containing whole inactivated influenza virus (WIIV) and a mucoadhesive compound suitable for nasal delivery. Powders containing WIIV and either lactose or trehalose were produced by lyophilization. A micro-ball mill was used to reduce the lyophilized cake to sizes suitable for nasal delivery. Chitosan flakes were reduced in size using a cryo-milling technique. Milled powders were sieved between 45 and 125 microm aggregate sizes and characterized for particle size and distribution, morphology, and flow properties. Powders were blended in the micro-ball mill without the ball. Lyophilization followed by milling produced irregularly shaped, polydisperse particles with a median primary particle diameter of approximately 21 microm and a yield of approximately 37% of particles in the 45 to 125 microm particle size range. Flow properties of lactose and trehalose powders after lyophilization followed by milling and sieving were similar. Cryo-milling produced a small yield of particles in the desired size range (<10%). Lyophilization followed by milling and sieving produced particles suitable for nasal delivery with different physicochemical properties as a function of processing conditions and components of the formulation. Further optimization of particle size and morphology is required for these powders to be suitable for clinical evaluation.

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.

A study of processing parameters in thermal-sprayed alumina and zircon mixtures

NASA Astrophysics Data System (ADS)

Li, Y.; Khor, K. A.

2002-06-01

A method of plasma spraying of alumina and zircon mixtures to form ZrO2-mullite composites has been proposed and developed. The feedstock is prepared by a combination of mechanical alloying, which allows formation of fine-grained, homogeneous solid-solution mixtures, followed by plasma spheroidization that yields rapid solidified microstructures and enhanced compositional homogeneity. The effects of ball-milling duration and milling media were studied. It was found that zirconia is a more efficient milling media and that increasing milling duration enhanced the dissociation of zircon. Flame spray and plasma spray processes were used to spheroidize the spray-dried powders. The temperature of the flame spray was found to be insufficient to melt the powders completely. The processing parameters of the plasma spray played an important role in zircon decomposition and mullite formation. Increasing the arc current or reducing secondary gas pressure caused more zircon to decompose and more mullite to form after heat treatment at 1200 °C for 3 h. Dissociation of zircon and the amount of mullite for med can be enhanced significantly when using the more efficient, computerized plasma-spraying system and increasing the ball-milling duration from 4 to 8 h.

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

Synthesis of TiCr2 intermetallic compound from mechanically activated starting powders via calcio-thermic co-reduction

NASA Astrophysics Data System (ADS)

Bayat, O.; Khavandi, A. R.; Ghasemzadeh, R.

2017-05-01

Effect of mechanical activation of TiO2 and Cr2O3 oxides as starting materials was investigated for direct synthesis of TiCr2. Differential thermal analysis (DTA) indicated that increasing the ball milling time resulted in lower exothermic reaction temperatures between molten Ca-Cr2O3 and molten Ca-TiO2. A model-free Kissinger type method was applied to DTA data to evaluate the reaction kinetics. The results reveal that the activation energy of the exothermic reactions decreased with increasing the milling time. The structure, oxygen content, and average particle sizes of the obtained TiCr2 product were affected by the ball milling time of the starting materials. Increasing the milling time from 10 to 40 h decreased the average particle size and oxygen content of the obtained TiCr2 from 10 to 2 μm and from 1690 to 1290 ppm, respectively. The X-ray diffraction (XRD) results showed that TiCr2 compounds with metastable bcc phase can be produced using nano-sized starting materials, while only a slight amount of bcc phase can be obtained in the TiCr2 compounds, using micron-sized starting materials. The TiCr2 obtained by this method had a hydrogen absorption capability of 0.63 wt % and the kinetics of the hydrogen absorption increased for the 40 h milled sample.

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.

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.

Amorphization of the prototypical zeolitic imidazolate framework ZIF-8 by ball-milling.

PubMed

Cao, Shuai; Bennett, Thomas D; Keen, David A; Goodwin, Andrew L; Cheetham, Anthony K

2012-08-14

We report the rapid amorphization of the prototypical substituted zeolitic imidazolate framework, ZIF-8, by ball-milling. The resultant amorphous ZIF-8 (a(m)ZIF-8) possesses a continuous random network (CRN) topology with a higher density and a lower porosity than its crystalline counterpart. A decrease in thermal stability upon amorphization is also evident.

Effect of sample preparation method on quantification of polymorphs using PXRD.

PubMed

Alam, Shahnwaz; Patel, Sarsvatkumar; Bansal, Arvind Kumar

2010-01-01

The purpose of this study was to improve the sensitivity and accuracy of quantitative analysis of polymorphic mixtures. Various techniques such as hand grinding and mixing (in mortar and pestle), air jet milling and ball milling for micronization of particle and mixing were used to prepare binary mixtures. Using these techniques, mixtures of form I and form II of clopidogrel bisulphate were prepared in various proportions from 0-5% w/w of form I in form II and subjected to x-ray powder diffraction analysis. In order to obtain good resolution in minimum time, step time and step size were varied to optimize scan rate. Among the six combinations, step size of 0.05 degrees with step time of 5 s demonstrated identification of maximum characteristic peaks of form I in form II. Data obtained from samples prepared using both grinding and mixing in ball mill showed good analytical sensitivity and accuracy compared to other methods. Powder x-ray diffraction method was reproducible, precise with LOD of 0.29% and LOQ of 0.91%. Validation results showed excellent correlation between actual and predicted concentration with R2 > 0.9999.

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

Grinding Si3N4 Powder In Si3N4 Equipment

NASA Technical Reports Server (NTRS)

Herbell, Thomas P.; Freedman, Marc R.; Kiser, James D.

1989-01-01

Three methods of grinding compared. Report based on study of grinding silicon nitride powder in preparation for sintering into solid ceramic material. Attrition, vibratory, and ball mills lined with reaction-bonded silicon nitride tested. Rates of reduction of particle sizes and changes in chemical compositions of powders measured so grinding efficiences and increases in impurity contents from wear of mills and media evaluated for each technique.

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.

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.

Solvent-free mechanochemical preparation of phosphonium salts, phosphorus ylides, and olefins

DOEpatents

Pecharsky, Vitalij K.; Balema, Viktor P.; Wiench, Jerzy W.; Pruski, Marek

2004-05-04

The present invention provides a method of preparing a phosphonium salt of the formula [R.sup.1 R.sup.2 R.sup.3 P--CR.sup.4 R.sup.5 R.sup.6 ]X, comprising ball-milling a phosphine of the formula R.sup.1 R.sup.2 R.sup.3 P with a compound of the formula XCR.sup.4 R.sup.5 R.sup.6 ; a method of preparing a phosphorus ylide of the formula R.sup.1 R.sup.2 R.sup.3 P.dbd.CR.sup.4 R.sup.5, comprising ball-milling a phosphonium salt of the formula [R.sup.1 R.sup.2 R.sup.3 P--HCR.sup.4 R.sup.5 ]X in the presence of a base; and a method of preparing an olefin of the formula R.sup.4 R.sup.5 C.dbd.CR.sup.7 H or R.sup.4 R.sup.5 C.dbd.CR.sup.7 R.sup.8, comprising ball-milling a phosphorus ylide of the formula R.sup.1 R.sup.2 R.sup.3 P.dbd.CR.sup.4 R.sup.5 with a compound of the formula R.sup.7 C(O)H or R.sup.7 C(O)R.sup.8. The inventive method produces phosphonium salts and phosphorus ylides by mechanical processing solid reagents under solvent-free conditions. The advantages of the present invention over conventional solution methods, include: (1) extremely high selectivity; (2) high yields; (3) low processing temperatures; (4) simple and scalable reactions using commercially available equipment; and (5) the complete elimination of solvents from the reaction.

Effect of powder reactivity on fabrication and properties of NiAl/Al2O3 composite coated on cast iron using spark plasma sintering

NASA Astrophysics Data System (ADS)

Beyhaghi, Maryam; Kiani-Rashid, Ali-Reza; Kashefi, Mehrdad; Khaki, Jalil Vahdati; Jonsson, Stefan

2015-07-01

Powder mixtures of Ni, NiO and Al are ball milled for 1 and 10 h. X-ray diffractometry and differential thermal analysis show that while ball milling for 1 h produced mechanically activated powder; 10 h ball milling produced NiAl and Al2O3 phases. Dense NiAl/Al2O3 composite coatings are formed on gray cast iron substrate by spark plasma sintering (SPS) technique. The effect of powder reactivity on microstructure, hardness and scratch hardness of NiAl/Al2O3 coatings after SPS is discussed. Results show that in the coating sample made of mechanically activated powder in situ synthesis of NiAl/Al2O3 composite coating is fulfilled and a thicker well-formed diffusion bond layer at the interface between coating and substrate is observed. The diffusion of elements across the bond layers and phase evolution in the bond layers were investigated. No pores or cracks were observed at the interface between coating layer and substrate in any of samples. Higher Vickers hardness and scratch hardness values in coating made of 10 h ball milled powder than in coating fabricated from 1 h ball milled powder are attributed to better dispersion of Al2O3 reinforcement particles in NiAl matrix and nano-crystalline structure of NiAl matrix. Scratched surface of coatings did not reveal any cracking or spallation at coating-substrate interface indicating their good adherence at test conditions.

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.

Effect of process control agent on the porous structure and mechanical properties of a biomedical Ti-Sn-Nb alloy produced by powder metallurgy.

PubMed

Nouri, A; Hodgson, P D; Wen, C E

2010-04-01

The influence of different amounts and types of process control agent (PCA), i.e., stearic acid and ethylene bis-stearamide, on the porous structure and mechanical properties of a biomedical Ti-16Sn-4Nb (wt.%) alloy was investigated. Alloy synthesis was performed on elemental metal powders using high-energy ball milling for 5h. Results indicated that varying the PCA content during ball milling led to a drastic change in morphology and particle-size distribution of the ball-milled powders. Porous titanium alloy samples sintered from the powders ball milled with the addition of various amounts of PCA also revealed different pore morphology and porosity. The Vickers hardness of the sintered titanium alloy samples exhibited a considerable increase with increasing PCA content. Moreover, the addition of larger amounts of PCA in the powder mixture resulted in a significant increase in the elastic modulus and peak stress for the sintered porous titanium alloy samples under compression. It should also be mentioned that the addition of PCA introduced contamination (mainly carbon and oxygen) into the sintered porous product. Crown Copyright 2009. Published by Elsevier Ltd. All rights reserved.

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.

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.

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.

Mechanochemical Synthesis and Thermoelectric Properties of Magnesium Silicide and Related Alloys

NASA Technical Reports Server (NTRS)

Bux, Sabah K. (Inventor); Fleurial, Jean-Pierre (Inventor); Kaner, Richard B. (Inventor)

2013-01-01

The present invention provides a method of making a substantially phase pure compound including a cation and an anion. The compound is made by mixing in a ball-milling device a first amount of the anion with a first amount of the cation that is less than the stoichiometric amount of the cation, so that substantially all of the first amount of the cation is consumed. The compound is further made by mixing in a ball-milling device a second amount of the cation that is less than the stoichiometric amount of the cation with the mixture remaining in the device. The mixing is continued until substantially all of the second amount of the cation and any unreacted portion of anion X are consumed to afford the substantially phase pure compound.

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.

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.

Effects of grinding processes on enzymatic degradation of wheat straw.

PubMed

Silva, Gabriela Ghizzi D; Couturier, Marie; Berrin, Jean-Guy; Buléon, Alain; Rouau, Xavier

2012-01-01

The effectiveness of wheat straw fine to ultra-fine grindings at pilot scale was studied. The produced powders were characterised by their particle-size distribution (laser diffraction), crystallinity (WAXS) and enzymatic degradability (Trichoderma reesei enzymatic cocktail). A large range of wheat-straw powders was produced: from coarse (median particle size ∼800 μm) to fine particles (∼50 μm) using sieve-based grindings, then ultra-fine particles ∼20 μm by jet milling and ∼10 μm by ball milling. The wheat straw degradability was enhanced by the decrease of particle size until a limit: ∼100 μm, up to 36% total carbohydrate and 40% glucose hydrolysis yields. Ball milling samples overcame this limit up to 46% total carbohydrate and 72% glucose yields as a consequence of cellulose crystallinity reduction (from 22% to 13%). Ball milling appeared to be an effective pretreatment with similar glucose yield and superior carbohydrate yield compared to steam explosion pretreatment. Copyright © 2011 Elsevier Ltd. All rights reserved.

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.

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

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.

From Si wafers to cheap and efficient Si electrodes for Li-ion batteries

NASA Astrophysics Data System (ADS)

Gauthier, Magali; Reyter, David; Mazouzi, Driss; Moreau, Philippe; Guyomard, Dominique; Lestriez, Bernard; Roué, Lionel

2014-06-01

High-energy ball milling is used to recycle Si wafers to produce Si powders for negative electrodes of Li-ion batteries. The resulting Si powder consists in micrometric Si agglomerates made of cold-welded submicrometric nanocrystalline Si particles. Silicon-based composite electrodes prepared with ball-milled Si wafer can achieve more than 900 cycles with a capacity of 1200 mAh g-1 of Si (880 mAh g-1 of electrode) and a coulombic efficiency higher than 99%. This excellent electrochemical performance lies in the use of nanostructured Si produced by ball milling, the electrode formulation in a pH 3 buffer solution with CMC as binder and the use of FEC/VC additives in the electrolyte. This work opens the way to an economically attractive recycling of Si wastes.

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.

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.

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.

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.

Production of ultra-thin nano-scaled graphene platelets from meso-carbon micro-beads

DOEpatents

Zhamu, Aruna; Guo, Jiusheng; Jang, Bor Z

2014-11-11

A method of producing nano-scaled graphene platelets (NGPs) having an average thickness no greater than 50 nm, typically less than 2 nm, and, in many cases, no greater than 1 nm. The method comprises (a) intercalating a supply of meso-carbon microbeads (MCMBs) to produce intercalated MCMBs; and (b) exfoliating the intercalated MCMBs at a temperature and a pressure for a sufficient period of time to produce the desired NGPs. Optionally, the exfoliated product may be subjected to a mechanical shearing treatment, such as air milling, air jet milling, ball milling, pressurized fluid milling, rotating-blade grinding, or ultrasonicating. The NGPs are excellent reinforcement fillers for a range of matrix materials to produce nanocomposites. Nano-scaled graphene platelets are much lower-cost alternatives to carbon nano-tubes or carbon nano-fibers.

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.

Size and morphology controlled NiSe nanoparticles as efficient catalyst for the reduction reactions

NASA Astrophysics Data System (ADS)

Subbarao, Udumula; Marakatti, Vijaykumar S.; Amshumali, Mungalimane K.; Loukya, B.; Singh, Dheeraj Kumar; Datta, Ranjan; Peter, Sebastian C.

2016-12-01

Facile and efficient ball milling and polyol methods were employed for the synthesis of nickel selenide (NiSe) nanoparticle. The particle size of the NiSe nanoparticle has been controlled mechanically by varying the ball size in the milling process. The role of the surfactants in the formation of various morphologies was studied. The compounds were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray energy dispersive spectroscopy (EDS). The efficiency of the NiSe nanoparticle as a catalyst was tested for the reduction of para-nitroaniline (PNA) to para-phenyldiamine (PPD) and para-nitrophenol (PNP) to para-aminophenol (PAP) using NaBH4 as the reducing agent. Particle size, morphology and the presence of surfactant played a crucial role in the reduction process.

The Mechanical Properties and In Vitro Biocompatibility of PM-Fabricated Ti-28Nb-35.4Zr Alloy for Orthopedic Implant Applications.

PubMed

Xu, Wei; Li, Ming; Wen, Cuie; Lv, Shaomin; Liu, Chengcheng; Lu, Xin; Qu, Xuanhui

2018-03-30

A biocompatible Ti-28Nb-35.4Zr alloy used as bone implant was fabricated through the powder metallurgy process. The effects of mechanical milling and sintering temperatures on the microstructure and mechanical properties were investigated systematically, before in vitro biocompatibility of full dense Ti-28Nb-35.4Zr alloy was evaluated by cytotoxicity tests. The results show that the mechanical milling and sintering temperatures have significantly effects on the density and mechanical properties of the alloys. The relative density of the alloy fabricated by the atomized powders at 1500 °C is only 83 ± 1.8%, while the relative density of the alloy fabricated by the ball-milled powders can rapidly reach at 96.4 ± 1.3% at 1500 °C. When the temperature was increased to 1550 °C, the alloy fabricated by ball-milled powders achieve full density (relative density is 98.1 ± 1.2%). The PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C can achieve a wide range of mechanical properties, with a compressive yield strength of 1058 ± 35.1 MPa, elastic modulus of 50.8 ± 3.9 GPa, and hardness of 65.8 ± 1.5 HRA. The in vitro cytotoxicity test suggests that the PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C has no adverse effects on MC3T3-E1 cells with cytotoxicity ranking of 0 grade, which is nearly close to ELI Ti-6Al-4V or CP Ti. These properties and the net-shape manufacturability makes PM-fabricated Ti-28Nb-35.4Zr alloy a low-cost, highly-biocompatible, Ti-based biomedical alloy.

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.

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.

Injection molding ceramics to high green densities

NASA Technical Reports Server (NTRS)

Mangels, J. A.; Williams, R. M.

1983-01-01

The injection molding behavior of a concentrated suspension of Si powder in wax was studied. It was found that the injection molding behavior was a function of the processing techniques used to generate the powder. Dry ball-milled powders had the best molding behavior, while air classified and impact-milled powders demonstrated poorer injection moldability. The relative viscosity of these molding batches was studied as a function of powder properties: distribution shape, surface area, packing density, and particle morphology. The experimental behavior, in all cases, followed existing theories. The relative viscosity of an injection molding composition composed of dry ball-milled powders could be expressed using Farris' relation.

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.

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.

A Science-Based Understanding of Cermet Processing

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

Cesarano, III, Joseph; Roach, Robert Allen; Kilgo, Alice C.

2006-04-01

This report is a summary of the work completed in FY01 for science-based characterization of the processes used to fabricate 1) cermet vias in source feedthrus using slurry and paste-filling techniques and 2) cermet powder for dry pressing. Common defects found in cermet vias were characterized based on the ability of subsequent processing techniques (isopressing and firing) to remove the defects. Non-aqueous spray drying and mist granulation techniques were explored as alternative methods of creating CND50, the powder commonly used for dry pressed parts. Compaction and flow characteristics of these techniques were analyzed and compared to standard dry-ball-milled CND50. Duemore » to processing changes, changes in microstructure can occur. A microstructure characterization technique was developed to numerically describe cermet microstructure. Machining and electrical properties of dry pressed parts were also analyzed and related to microstructure using this analytical technique.3 Executive SummaryThis report outlines accomplishments in the science-based understanding of cermet processing up to fiscal year 2002 for Sandia National Laboratories. The three main areas of work are centered on 1) increasing production yields of slurry-filled cermets, 2) evaluating the viability of high-solids-loading pastes for the same cermet components, and 3) optimizing cermet powder used in pressing processes (CND50). An additional development that was created as a result of the effort to fully understand the impacts of alternative processing techniques is the use of analytical methods to relate microstructure to physical properties. Recommendations are suggested at the end of this report. Summaries of these four efforts are as follows:1.Increase Production Yields of Slurry-Filled Cermet Vias Finalized slurry filling criteria were determined based on three designs of experiments where the following factors were analyzed: vacuum time, solids loading, pressure drop across the filter paper, slurry injection rate, via prewetting, slurry injection angle, filter paper prewetting, and slurry mixing time. Many of these factors did not have an influence on defect formation. In order of decreasing importance, critical factors for defect formation by slurry filling are vacuum time (20 sec. optimal), slurry solids loading (20.0 g of cermet with 13.00 g of DGBEA solvent (21.2 vol%)), filling with the pipette in a vertical position, and faster injection rates (%7E765 l/s) as preferable to slower. No further recommendations for improvement to this process can be suggested. All findings of the slurry filling process have been transferred to CeramTec, the supplier. Paste filling methods appear to show more promise of increasing production yields. The types of flaws commonly found in slurry-filled vias were identified and followed throughout the entire source feedthru process. In general, all sizes of cracks healed during isopressing and firing steps. Additionally, small to medium sized voids (less than 1/3 the via diameter) can be healed. Porosity will usually lead to via necking, which may cause the part to be out of specification. Large voids (greater 4 than 1/3 of the diameter) and partial fills are not healed or produce significant necking. 2.Viability of High-Solids-Loading-Cermet Paste for Filling Source Feedthru ViaThe paste-filling process is easy to implement and easier to use. The high solids loading (>40 vol %) reduces the incidence of drying defects, which are seen in slurry filled (%7E23 vol %) vias. Additionally, the way in which the vias are filled (the paste is pushed from entrance to exit, displacing air as the paste front progresses), reduces the chance of entrapped voids, which are common in the slurry filling process. From the fair number of samples already filled, the likelihood of this process being a viable and reliable process is very good. Issues of concern for the paste process, as with any new process, are any problems that may arise in subsequent manufacturing stages of the neutron tube that may be affected by subtle changes in microstructure. Both MC4277 and MC4300-type source feedthrus were paste-filled by hand. X-ray analysis showed a much lower existence of voids in the green parts as compared to slurry-filled parts. The paste shows improvements in shelf life (weeks) as compared to slurry (minutes). This method of introducing the cermet to the via also lends itself very well to an automated filling process where a machine can either drill vias or, with the aid of a vision system, find pre-drilled vias and fill them with paste. The pastes used in this work prove the concept of this automated filling process as MC4277 sources have been filled using such a prototype machine, however, better performing pastes can be developed which are less hazardous (aqueous systems). The paste process was also used to successfully fill MC4300 "dogleg" type sources.3.Optimize CND50 Two methods of creating granulated cermet powder for comparison with dry-ball milled CND50 were explored. The first method, non-aqueous spray drying, was performed at Niro Inc. used a 40/60 (wt %) ethanol/toluene solvent and three binder systems; polyvinyl butyral (B79), ethylcellulose (Ethocel), and hydroxypropylcellulose (Klucel). Due to the nature of small spray-dry systems, an excess amount of fines was present in the granulated powder, which may have contributed to the low angles of repose (68 to 78). This is a moderate increase in 5 flowability as standard dry-ball milled powder possesses an angle of repose of 79-89. Mist granulated powders were produced with a tert-butanol solvent and polyvinyl butyral binder system. The angles of repose were more promising (28). More investigation into the mist granulation method is required. Also, aqueous spray drying may be possible with cermet and should be explored. Compaction of all granulated powders is much closer to a proven pressing powder (Sandi94 - angle of repose 29) which should allow cermet to be pressed to near net shape where die filling is difficult for non-flowing powders.4.Microstructure Characterization An analytical technique was developed to numerically characterize microstructures in terms of molybdenum dispersion, homogeneity, and percolation indices. This technique was applied to dry-ball-milled samples of various ball-milling times (0.5 to 20 hours). Significant change in the microstructure could be seen with milling time. Increased milling time caused agglomeration of molybdenum particles, increasing the percolation index, whereas short milling times promoted higher dispersion indices. This phenomenon is contrary to conventional understanding of mixing. However, conventional ball milling does not usually incorporate granules with binder and separate particles. This discrepancy may explain the odd mixing behavior. It is important to note that the high percolation index possessed by long ball mill times showed lower electrical resistance than low-percolation-index microstructures. However, machinability of high percolation, low-dispersion-index microstructures were poor as compared to microstructures with high dispersion indices and moderate percolation indices. This trade-off between dispersion and percolation (at constant molybdenum levels) suggests that microstructures can be achieved that posses good mechanical and electrical properties. Coincidentally, microstructures that satisfy this condition are produced by the standard dry-ball-milled CND50 (4 hour ball mill time). The performance and sensitivity of the microstructure characterization technique should be evaluated, specifically for electrical conductivity. Processing techniques to decrease the percolation index (lowering molybdenum content, excess ball milling, 6 larger molybdenum particles, etc.) should be employed to determine the point where cermet is not conductive or falls below electrical conduction specifications.7« less

Dry mechanochemical synthesis of hydroxyapatites from DCPD and CaO: influence of instrumental parameters on the reaction kinetics.

PubMed

Mochales, Carolina; El Briak-BenAbdeslam, Hassane; Ginebra, Maria Pau; Terol, Alain; Planell, Josep A; Boudeville, Philippe

2004-01-01

Mechanochemistry is a possible route to synthesize calcium deficient hydroxyapatite (CDHA) with an expected molar calcium-to-phosphate (Ca/P) ratio +/-0.01. To optimize the experimental conditions of CDHA preparation from dicalcium phosphate dihydrate (DCPD) and calcium oxide by dry mechanosynthesis reaction, we performed the kinetic study varying some experimental parameters. This kinetic study was carried out with two different planetary ball mills (Retsch or Fritsch Instuments). Results obtained with the two mills led to the same conclusions although the values of the rate constants of DCPD disappearance and times for complete reaction were very different. Certainly, the origin of these differences was from the mills used, thus we investigated the influence of instrumental parameters such as the mass and the surface area of the balls or the rotation velocity on the mechanochemical reaction kinetics of DCPD with CaO. Results show that the DCPD reaction rate constant and the inverse of the time for complete disappearance of CaO both vary linearly with (i) the square of the rotation velocity, (ii) the square of eccentricity of the vial on the rotating disc and (iii) the product of the mass by the surface area of the balls. These observations comply with theoretical models developed for mechanical alloying. The consideration of these four parameters allows the transposition of experimental conditions from one mill to another or the comparison between results obtained with different planetary ball mills. These instrumental parameters have to be well described in papers concerning mechanochemistry or when grinding is an important stage in a process.

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.

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

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti{sub 55}C{sub 45} bulk material

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

Sherif El-Eskandarany, M., E-mail: msherif@kisr.edu.kw; Al-Hazza, Abdulsalam

2014-11-15

We employed a high-energy ball mill for the synthesis of nanograined Ti{sub 55}C{sub 45} powders starting from elemental Ti and C powders. The mechanically induced self-propagating reaction that occurred between the reactant materials was monitored via a gas atmosphere gas-temperature-monitoring system. A single phase of NaCl-type TiC was obtained after 5 h of ball milling. To decrease the powder and grain sizes, the material was subjected to further ball milling time. The powders obtained after 200 h of milling possessed spherical-like morphology with average particle and grain sizes of 45 μm and 4.2 nm, respectively. The end-products obtained after 200more » h of ball milling time, were then consolidated into full dense compacts, using hot pressing and spark plasma sintering at 1500 and 34.5 MPa, with heating rates of 20 °C/min and 500 °C/min, respectively. Whereas hot pressing of the powders led to severe grain growth (∼ 436 nm in diameter), the as-spark plasma sintered powders maintained their nanograined characteristics (∼ 28 nm in diameter). The as-synthesized and as-consolidated powders were characterized, using X-ray diffraction, high-resolution electron microscopy, and scanning electron microscopy. The mechanical properties of the consolidated samples obtained via the hot pressing and spark plasma sintering techniques were characterized, using Vickers microhardness and non-destructive testing techniques. The Vickers hardness, Young's modulus, shear modulus and fracture toughness of as-spark plasma sintered samples were 32 GPa, 358 GPa, 151 GPa and 6.4 MPa·m{sup 1/2}, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed. - Highlights: • Room-temperature synthesizing of NaCl-type TiC • Dependence on the grain size on the ball milling time • Fabrication of equiaxed nanocrystalline grains with a diameter of 4.2 nm • Fabrication of nanocrystalline bulk TiC material by SPS with minimal grain growth • Dependence of improved mechanical properties on the consolidation techniques.« less

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

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.

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

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

NASA Astrophysics Data System (ADS)

Santhanam, Priya Radhi

Mechanical milling is a widely used technique for powder processing in various areas. In this work, a scale-up model for describing this ball milling process is developed. The thesis is a combination of experimental and modeling efforts. Initially, Discrete Element Model (DEM) is used to describe energy transfer from milling tools to the milled powder for shaker, planetary, and attritor mills. The rolling and static friction coefficients are determined experimentally. Computations predict a quasisteady rate of energy dissipation, E d, for each experimental configuration. It is proposed that the milling dose defined as a product of Ed and milling time, t, divided by the mass of milled powder, mp characterizes the milling progress independently of the milling device or milling conditions used. Once the milling dose is determined for one experimental configuration, it can be used to predict the milling time required to prepare the same material in any milling configuration, for which Ed is calculated. The concept is validated experimentally for DEM describing planetary and shaker mills. For attritor, the predicted Ed includes substantial contribution from milling tool interaction events with abnormally high forces (>103 N). The energy in such events is likely dissipated to heat or plastically deform milling tools rather than refine material. Indeed, DEM predictions for the attritor correlate with experiments when such events are ignored in the analysis. With an objective of obtaining real-time indicators of milling progress, power, torque, and rotation speed of the impeller of an attritor mill are measured during preparation of metal matrix composite powders in the subsequent portion of this thesis. Two material systems are selected and comparisons made between in-situ parameters and experimental milling progress indicators. It is established that real-time measurements can certainly be used to describe milling progress. However, they need to be interpreted carefully 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.

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.

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.

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.

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

The Mechanical Properties and In Vitro Biocompatibility of PM-Fabricated Ti-28Nb-35.4Zr Alloy for Orthopedic Implant Applications

PubMed Central

Xu, Wei; Li, Ming; Wen, Cuie; Lv, Shaomin; Liu, Chengcheng; Lu, Xin

2018-01-01

A biocompatible Ti-28Nb-35.4Zr alloy used as bone implant was fabricated through the powder metallurgy process. The effects of mechanical milling and sintering temperatures on the microstructure and mechanical properties were investigated systematically, before in vitro biocompatibility of full dense Ti-28Nb-35.4Zr alloy was evaluated by cytotoxicity tests. The results show that the mechanical milling and sintering temperatures have significantly effects on the density and mechanical properties of the alloys. The relative density of the alloy fabricated by the atomized powders at 1500 °C is only 83 ± 1.8%, while the relative density of the alloy fabricated by the ball-milled powders can rapidly reach at 96.4 ± 1.3% at 1500 °C. When the temperature was increased to 1550 °C, the alloy fabricated by ball-milled powders achieve full density (relative density is 98.1 ± 1.2%). The PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C can achieve a wide range of mechanical properties, with a compressive yield strength of 1058 ± 35.1 MPa, elastic modulus of 50.8 ± 3.9 GPa, and hardness of 65.8 ± 1.5 HRA. The in vitro cytotoxicity test suggests that the PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C has no adverse effects on MC3T3-E1 cells with cytotoxicity ranking of 0 grade, which is nearly close to ELI Ti-6Al-4V or CP Ti. These properties and the net-shape manufacturability makes PM-fabricated Ti-28Nb-35.4Zr alloy a low-cost, highly-biocompatible, Ti-based biomedical alloy. PMID:29601517

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%.

Atomic disorder, phase transformation, and phase restoration in Co3Sn2

NASA Astrophysics Data System (ADS)

di, L. M.; Zhou, G. F.; Bakker, H.

1993-03-01

The behavior of the intermetallic compound Co3Sn2 upon ball milling was studied by x-ray diffraction, high-field-magnetization measurements, and subsequently by differential scanning calorimetry. It turns out that starting from the stoichiometric-ordered compound, mechanical attrition of Co3Sn2 generates atomic disorder in the early stage of milling. The nonequilibrium phase transformation from the low-temperature phase with orthorhombic structure to the high-temperature phase with a hexagonal structure was observed in the intermediate stage of milling. It was accompanied by the creation of increasing atomic disorder. After long milling periods, the phase transformation was completed and the atomic disordering became saturated. All the physical parameters measured in the present work remained constant during this period. The above outcome was confirmed by comparison with the high-temperature phase thermally induced by quenching. The good agreement of the results obtained by different techniques proves that the ball milling generates well-defined metastable states in Co3Sn2.

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.

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 %.

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.

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.

Compressive Deformation Behavior of Open-Cell Cu-Zn-Al Alloy Foam Made Through P/M Route Using Mechanically Alloyed Powder

NASA Astrophysics Data System (ADS)

Barnwal, Ajay Kumar; Mondal, D. P.; Kumar, Rajeev; Prasanth, N.; Dasgupta, R.

2018-03-01

Cu-Zn-Al foams of varying porosity fractions using mechanical alloyed powder have been made through powder metallurgy route. Here, NH4 (HCO3) was used as a space holder. Mechanically alloyed Cu-Zn-Al is made using a planetary ball mill taking the ratio of Cu/Zn/Al = 70:25:5 (by weight ratio). The ball/powder ratios were varied in the four ranges 10:1, 15:1, 20:1, and 25:1. Green compacts of milled powder and space holder samples were sintered at three stages at three different temperatures 350, 550, and 850 °C for 1 h at each stage. The crystalline size and particle size as a function of ball/powder ratios were examined. The compressive deformation responses of foams are varied with relative density and the ball/powder ratio. The plateau stress and energy absorption of these foams increase with an increase in relative density but decreases with increase in ball/powder ratio, even though crystalline size decreases. This has further been explained on the basis of particle morphology as a function of ball/powder ratio.

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.

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.

Study of microforging of metallic nanoflakes in relation to electronic applications

NASA Astrophysics Data System (ADS)

Kang, Wooseung

This dissertation reports the first systematic study of cold microforging; the conversion of micron scale metal powders to thin flakes by a series of plastically deforming impacts in a ball mill at low temperature. The research focused on processing Fe and Cu flakes with submicron thicknesses (nanoflakes) which are expected to find significant applications in electronics. The principal objectives were to develop a detailed understanding of the underlying materials science of the process, and to characterize the material and processing parameters that maximize the rate at which nanoflakes with a specific aspect ratio (diameter/thickness) can be microforged. A model for microforging was developed using Hertzian impact theory to establish the compressive impact energy (Emf) imparted to a spherical powder particle in a ball-powder-ball impact, and the Coffin-Manson relation for cyclical fatigue to determine the number of plastically deforming impacts it could sustain before fracturing. The rate of microforging in the ball mill was obtained from the product of the impact frequency (f) and the statistical probability of impact (p). Both f and p depend on the number of balls and powders, and the collision velocity (v) and the milling vial volume (V). The parameters Emf, p, v and V are specific to the mill and used to develop scaling laws for transferring the process from small vibratory research mills to large commercial equipment. The empirical parameters required by these models were determined by microforging a few grams of powders in small research mills. The validity of the model was assessed by comparing the time required to microforge several hundred grams of a particular powder in a much larger mill, with that determined by scaling the model equations to account for change in mill parameters. The good agreement obtained provided strong support for the microforging model. SEM microphotos and sieving fractions were used to show that the minimum thicknesses, and maximum aspect ratios of the Fe and Cu nanoflakes that could be produced before fracture, are in the ~0.3 μm-0.5 μm range, and agreed well with those calculated from volume conserving sphere-flake transformations. X-ray diffraction measurements showed that the grain sizes of these powders were ~0.1x their thicknesses, and were little changed by microforging. The magnetic hysteresis and permeabilities of the Fe nanoflakes were in good agreement with those computed from the nanoflake geometries. The results indicate that the model of microforging as a statistical random sequence of plastic deformations can be used to develop a commercial process to support the development of their application potential in electronics.

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.

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.

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.

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.

High spatial resolution PEELS characterization of FeAl nanograins prepared by mechanical alloying

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

Valdre, G.; Botton, G.A.; Brown, L.M.

The authors investigate the nanograin ``chemical`` structure in a nanostructured material of possible industrial application (Fe-Al system) prepared by conventional mechanical alloying via ball milling in argon atmosphere. They restrict themselves to the structural and nanochemical behavior of ball-milled nanocrystalline Fe-Al powders with atomic composition Fe{sub 3}Al, corresponding to a well-known intermetallic compound of the Fe-Al system. Scanning transmission electron microscopy (STEM) equipped with a parallel detection electron energy loss spectrometer (PEELS) has provided an insight on the ``chemical`` structure of both nanograins and their surface at a spatial resolution of better than 1 nm. The energy loss near edgemore » structure of the Al L loss reveals that the Al coordination is similar to a B2 compound and the oxidation of the powder during processing may play a significant role in the stabilization of the intermetallic phases. Conventional transmission electron microscopy (TEM) was used for the structural characterization of the material after the ball milling; powder X-ray diffraction (XRD) aided the investigation.« less

Fabrication of stable electrode/diffusion barrier layers for thermoelectric filled skutterudite devices

DOEpatents

Jie, Qing; Ren, Zhifeng; Chen, Gang

2015-12-08

Disclosed are methods for the manufacture of n-type and p-type filled skutterudite thermoelectric legs of an electrical contact. A first material of CoSi.sub.2 and a dopant are ball-milled to form a first powder which is thermo-mechanically processed with a second powder of n-type skutterudite to form a n-type skutterudite layer disposed between a first layer and a third layer of the doped-CoSi.sub.2. In addition, a plurality of components such as iron, and nickel, and at least one of cobalt or chromium are ball-milled form a first powder that is thermo-mechanically processed with a p-type skutterudite layer to form a p-type skutterudite layer "second layer" disposed between a first and a third layer of the first powder. The specific contact resistance between the first layer and the skutterudite layer for both the n-type and the p-type skutterudites subsequent to hot-pressing is less than about 10.0 .mu..OMEGA.cm.sup.2.

Fabrication of stable electrode/diffusion barrier layers for thermoelectric filled skutterudite devices

DOEpatents

Jie, Qing; Ren, Zhifeng; Chen, Gang

2017-08-01

Disclosed are methods for the manufacture of n-type and p-type filled skutterudite thermoelectric legs of an electrical contact. A first material of CoSi.sub.2 and a dopant are ball-milled to form a first powder which is thermo-mechanically processed with a second powder of n-type skutterudite to form a n-type skutterudite layer disposed between a first layer and a third layer of the doped-CoSi.sub.2. In addition, a plurality of components such as iron, and nickel, and at least one of cobalt or chromium are ball-milled form a first powder that is thermo-mechanically processed with a p-type skutterudite layer to form a p-type skutterudite layer "second layer" disposed between a first and a third layer of the first powder. The specific contact resistance between the first layer and the skutterudite layer for both the n-type and the p-type skutterudites subsequent to hot-pressing is less than about 10.0 .mu..OMEGA.cm.sup.2.

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

Raj K. Rajamani; Jose Angel Delgadillo

A research team from the University of Utah is working to make inroads into saving energy in these SAG mills. In 2003, Industries of the Future Program of the Department of Energy tasked the University of Utah team to build a partnership between the University and the mining industry for the specific purpose of reducing energy consumption in SAG mills. A partnership was formed with Cortez Gold Mines, Kennecott Utah Copper Corporation, Process Engineering Resources Inc. and Outokumpu Technology. In the current project, Cortez Gold Mines played a key role in facilitating the 26-ft SAG mill at Cortez as amore » test mill for this study. According to plant personnel, there were a number of unscheduled shut downs to repair broken liners and the mill throughput fluctuated depending on ore type. The University team had two softwares, Millsoft and FlowMod to tackle the problem. Millsoft is capable of simulating the motion of charge in the mill. FlowMod calculates the slurry flow through the grate and pulp lifters. Based on this data the two models were fine-tuned to fit the Cortez SAG will. In the summer of 2004 a new design of shell lifters were presented to Cortez and in September 2004 these lifters were installed in the SAG mill. By December 2004 Cortez Mines realized that the SAG mill is drawing approximately 236-kW less power than before while maintaining the same level of production. In the first month there was extreme cycling and operators had to learn more. Now the power consumption is 0.3-1.3 kWh/ton lower than before. The actual SAG mill power draw is 230-370 kW lower. Mill runs 1 rpm lesser in speed on the average. The recirculation to the cone crusher is reduced by 1-10%, which means more efficient grinding of critical size material is taking place in the mill. All of the savings have resulted in reduction of operating cost be about $0.023-$0.048/ ton. After completing the shell lifter design, the pulp lifter design was taken up. Through a series of mill surveys and model calculations it was figured that the radial pulp lifter installed on the mill had less than optimum discharge capacity. A number of alternative designs were evaluated. The final choice was the Turbo Pulp Lifter for which Outukumpu Technology, Centennial, Colorado had filed a patent. After installation of the pulp lifter a 22% increase in throughput rate from 344 stph to 421 stph was realized. A 35% decrease in the SAG mill power draw from 3,908 HP to 2,526 HP (2,915 kW to 1,884 kW) was recorded. This equates to a 47% decrease in SAG unit energy consumption from 8.98 kWh/ton to 4.74 kWh/ton. A 11% decrease in SAG mill speed was observed indicating optimized ball strikes. Also, the ball chip generation from the SAG mill was reduced considerably. Further more, a 7% decrease in ball mill power draw from 4,843 HP to 4,491 HP (3,613 kW to 3,350 kW) was observed. This equates to a 24% decrease in ball mill unit energy consumption from 11.13 kWh/ton to 8.43 kWh/ton.« less

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

Influence of temperature on AC conductivity of nanocrystalline CuAlO2

NASA Astrophysics Data System (ADS)

Prakash, T.

2012-07-01

Nanocrystalline CuAlO2 was synthesized by mechanical alloying of Cu2O and α-Al2O3 powders in the molar ratio of 1:1 for 20 h in toluene medium with tungsten carbide balls and vials using planetary ball mill. The ball milling was carried out at 300 rpm with a ball to powder weight ratio of 10:1 and then annealed at 1373 K in a platinum crucible for 20 h to get CuAlO2 phase with average crystallite size 45 nm. Complex impedance spectroscopic measurement in the frequency region 1 Hz to 10 MHz between the temperatures 333 to 473 K was carried out for nanocrystalline CuAlO2 sample. The obtained complex impedance data was analyzed for AC conductivities, DC and AC conductivities correlations and crossover frequencies ( f co ). The BNN (Barton, Nakajima and Namikawa) relation was applied to understand the correlation between DC and AC conductivities. The observed experimental results were discussed in the paper.

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.

Grain refinement and Lattice Imperfections in Commercial Aluminum Alloy Processed by Severe Plastic Deformation

NASA Astrophysics Data System (ADS)

Charfeddine, Saifeddine; Zehani, Karim; Besais, Lotfi; Korchef, Atef

2014-08-01

In the present work, investigations on the microstructure of an aluminum alloy that had been subjected to severe plastic deformation (SPD) by equal channel angular pressing (ECAP), filing and ball milling, were carried out using X-ray diffraction and scanning electron microscopy. SPD leads to lattice distortions, increased dislocation density and an intensive refinement of the microstructure. The refinement and lattice imperfections of the material are greatly affected by the deformation modes and loading performance occurring during SPD. During the milling, the dislocation annihilation increases at higher strains thereby resulting in a smaller crystallite size. After ECAP, the material manifests a strong shear texture and anisotropy of the deformation behavior. Strain anisotropy is less pronounced in filed and ball milled powder particles.

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.

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

Synthesis of fcc Mg-Ti-H alloys by high energy ball milling: Structure and electrochemical hydrogen storage properties

NASA Astrophysics Data System (ADS)

Rousselot, Steeve; Guay, Daniel; Roué, Lionel

Mg-Ti-H alloys were synthesized by high energy ball milling from equimolar mixtures of MgH 2 + TiH 2, MgH 2 + Ti and Mg + TiH 2 in the presence of 10 wt.% Pd. X-ray diffraction analyses combined with Rietveld refinement revealed that after 60 h of milling, all as-milled Mg-Ti-H alloys are made of two face-centered-cubic (fcc) phases, with lattice parameters ∼4.47 and ∼4.25 Å, in different proportions depending on the composition of the initial mixture. The Mg-Ti-H alloys displayed a similar electrochemical behavior, i.e. their hydrogen discharge capacity was highest during the first cycle and then decreased rapidly with cycling. The maximum discharge capacities of the 60 h-milled MgH 2 + TiH 2, MgH 2 + Ti and Mg + TiH 2 materials were 300, 443 and 454 mAh g -1, respectively. No apparent correlation could be established between the maximum discharge capacity of the Mg-Ti-H materials and the two fcc phase proportion.

Powder metallurgy of Ge, Si, and Ge-Si

NASA Astrophysics Data System (ADS)

Schilz, Jürgen; Langenbach, Marion

1993-03-01

id="ab1"Planetary ball-milling and pressing behaviour of Ge, Si and Ge-Si powder mixtures are investigated. Scanning and transmission electron microscopy observations revealed the different microstructure of the two elements after milling: Ge remains in a microcrystalline state, whereas Si can be comminuted into grains consisting of nanocrystalline regions. Planetary milling of the two elements together, using agate balls and vial, did not reveal any compound formation. By hot-isostatic pressing, pure Ge and Ge-Si mixtures were densified to a higher value than pure Si. This denotes a plastic flow of the Ge component at a process temperature of 800°C. The microhardness of hot-pressed Ge reaches the bulk value; hot-pressed Si is very soft. Energy dispersive X-ray analysis and X-ray diffraction did not detect any impurity contamination from vial and milling media wear. Moreover, by electrical transport measurements it turned out that the net carrier concentration density resulting from electrical active impurities introduced by the milling and pressing process is below 2 x 1016 cm 3 at room temperature.

Non-aqueous solution preparation of doped and undoped lixmnyoz

DOEpatents

Boyle, Timothy J.; Voigt, James A.

1997-01-01

A method for generation of phase-pure doped and undoped Li.sub.x Mn.sub.y O.sub.z precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder.

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.

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.

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.

Formulation and Characterization of a Plasma Sterilized, Pharmaceutical Grade Chitosan Powder

PubMed Central

Crofton, Andrew R; Hudson, Samuel M; Howard, Kristy; Pender, Tyler; Abdelgawad, Abdelrahman; Wolski, Daniel; Kirsch, Wolff M

2016-01-01

Chitosan has great potential as a pharmaceutical excipient. In this study, chitosan flake was micronized using cryo-ball and cryo-jet milling and subsequently sterilized with nitrogen plasma. Micronized chitosan was characterized by laser diffraction, scanning electron microscopy (SEM), conductometric titration, viscometry, loss on drying, FTIR, and limulus amebocyte lysate (LAL) assays. Cryo-jet milling produced mean particle size of 16.05 μm, 44% smaller than cryo-ball milling. Cryomilled chitosan demonstrated increased hygroscopicity, but reduced molecular weight and degree of deacetylation (DD). SEM imaging showed highly irregular shapes. FTIR showed changes consistent with reduced DD and an unexplained shift at 1100 cm−1. Plasma treated chitosan was sterile with <2.5 EU/g after low-pressure plasma and <1.3 EU/g after atmospheric pressure plasma treatment. Plasma treatment decreased the reduced viscosity of chitosan flake and powder, with a greater effect on powder. In conclusion, pharmaceutical grade, sterile chitosan powder was produced with cryo-jet milling and plasma sterilization. PMID:27112892

Vanadium dioxide-based materials for potential thermal switching applications

NASA Astrophysics Data System (ADS)

Jeong, Minyoung

One of the materials able to exhibit a transition from insulators to metals (IMT materials) is vanadium dioxide (VO2). Through IMT, VO2 shows a drop of resistivity of five orders of magnitude at a picosecond timescale. In this work, the feasibility of using VO2 as an efficient thermal switching device is discussed. Several synthesis methods (sol-gel, hot press and spark plasma sintering) were attempted to obtain VO2 sample in pellet form. From the X-ray diffraction results, it was found that spark plasma sintering (SPS) yielded the highest phase purity. Several sintering parameters such as temperature or sintering time were tested to determine the optimal sintering conditions. For better thermal switching behavior, high-energy ball milling was used to reduce lattice thermal conductivity (klat.) in the insulator phase. Ball-milling time was varied from 30 minutes to 2 hours. It was found that with increasing milling time, the k lat. was reduced. Thus, it was demonstrated that thermal switching behavior was most efficient with 2 hour-milling. To improve electronic thermal conductivity ( kelec.) in the metallic state, nano-sized copper particles were added to the VO2 system with a subtle amount variation ranging from 3at % to 5 at%. Results show that a composite with 5 at% Cu (copper) addition exhibited the largest increase in thermal conductivity ( k) in the metallic state. In addition to this, a basic mechanism behind IMT and some of the exemplary IMT-based applications were introduced.

A Versatile Low Temperature Synthetic Route to Zintl Phase Precursors: Na4Si4, Na4Ge4 and K4Ge4 as Examples

PubMed Central

Ma, Xuchu; Xu, Fen; Atkins, Tonya; Goforth, Andrea M.; Neiner, Doinita; Navrotsky, Alexandra; Kauzlarich, Susan M.

2010-01-01

Na4Si4 and Na4Ge4 are ideal chemical precursors for inorganic clathrate structures, clusters, and nanocrystals. The monoclinic Zintl phases, Na4Si4 and Na4Ge4, contain isolated homo-tetrahedranide [Si4]4− and [Ge4]4− clusters surrounded by alkali metal cations. In this study, a simple scalable route has been applied to prepare Zintl phases of composition Na4Si4 and Na4Ge4 using the reaction between NaH and Si or Ge at low temperature (420 °C for Na4Si4 and 270 °C for Na4Ge4). The method was also applied to K4Ge4, using KH and Ge as raw materials, to show the versatility of this approach. The influence of specific reaction conditions on the purity of these Zintl phases has been studied by controlling five factors: the method of reagent mixing (manual or ball milled), the stoichiometry between raw materials, the reaction temperature, the heating time and the gas flow rate. Moderate ball-milling and excess NaH or KH facilitate the formation of pure Na4Si4, Na4Ge4 or K4Ge4 at 420 °C (Na4Si4) or 270 °C (both M4Ge4 compounds, M = Na, K). TG/DSC analysis of the reaction of NaH and Ge indicates that ball milling reduces the temperature for reaction and confirms the formation temperature. This method provides large quantities of high quality Na4Si4 and Na4Ge4 without the need for specialized laboratory equipment, such as Schlenk lines, niobium/tantalum containers, or an arc welder, thereby expanding the accessibility and chemical utility of these phases by making them more convenient to prepare. This new synthetic method may also be extended to lithium-containing Zintl phases (LiH is commercially available) as well as to alkali metal-tetrel Zintl compounds of other compositions, e.g. K4Ge9. PMID:19921060

Mechanical Properties of β-Ti-35Nb-2.5Sn Alloy Synthesized by Mechanical Alloying and Pulsed Current Activated Sintering

NASA Astrophysics Data System (ADS)

Omran, Abdel-Nasser; Woo, Kee-Do; Lee, Hyun Bom

2012-12-01

A developed Ti-35 pct Nb-2.5 pct Sn (wt pct) alloy was synthesized by mechanical alloying using high-energy ball-milled powders, and the powder consolidation was done by pulsed current activated sintering (PCAS). The starting powder materials were mixed for 24 hours and then milled by high-energy ball milling (HEBM) for 1, 4, and 12 hours. The bulk solid samples were fabricated by PCAS at 1073 K to 1373 K (800 °C to 1100 °C) for a short time, followed by rapid cooling to 773 K (500 °C). The relative density of the sintered samples was about 93 pct. The Ti was completely transformed from α to β-Ti phase after milling for 12 hours in powder state, and the specimen sintered at 1546 K (1273 °C) was almost transformed to β-Ti phase. The homogeneity of the sintered specimen increased with increasing milling time and sintering temperature, as did its hardness, reaching 400 HV after 12 hours of milling. The Young's modulus was almost constant for all sintered Ti-35 pct Nb-2.5 pct Sn specimens at different milling times. The Young's modulus was low (63.55 to 65.3 GPa) compared to that of the standard alloy of Ti-6Al-4V (100 GPa). The wear resistance of the sintered specimen increased with increasing milling time. The 12-hour milled powder exhibited the best wear resistance.

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.

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.

Rapid fabrication of miniature lens arrays by four-axis single point diamond machining

PubMed Central

McCall, Brian; Tkaczyk, Tomasz S.

2013-01-01

A novel method for fabricating lens arrays and other non-rotationally symmetric free-form optics is presented. This is a diamond machining technique using 4 controlled axes of motion – X, Y, Z, and C. As in 3-axis diamond micro-milling, a diamond ball endmill is mounted to the work spindle of a 4-axis ultra-precision computer numerical control (CNC) machine. Unlike 3-axis micro-milling, the C-axis is used to hold the cutting edge of the tool in contact with the lens surface for the entire cut. This allows the feed rates to be doubled compared to the current state of the art of micro-milling while producing an optically smooth surface with very low surface form error and exceptionally low radius error. PMID:23481813

Effects of the morphology of CIPs on microwave absorption behaviors

NASA Astrophysics Data System (ADS)

Woo, Soobin; Yoo, Chan-Sei; Kim, Hwijun; Lee, Mijung; Quevedo-Lopez, Manuel; Choi, Hyunjoo

2017-11-01

Electromagnetic (EM) wave absorption properties are affected by the thickness and surface area of absorbing materials. In this study, a facile ball-milling process was introduced to effectively reduce the diameter and increase the aspect ratio of carbonyl iron powder (CIP), which is one of the most commercially available EM-absorbing materials. The size, aspect ratio, and consequent surface area of CIP were manipulated by controlling the milling parameters to investigate their effects on EM absorption properties. The results indicated that ball-milled CIPs exhibited better EM wave absorption ability when compared with that of pristine CIPs. However, significant differences in minimum reflection loss values were not observed between CIPs with different morphologies and similar specific surface areas. Hence, both fine and flaky CIPs were considered as beneficial for EM wave absorption.[Figure not available: see fulltext.

Shale-oil-recovery systems incorporating ore beneficiation. Final report.

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

Weiss, M.A.; Klumpar, I.V.; Peterson, C.R.

This study analyzed the recovery of oil from oil shale by use of proposed systems which incorporate beneficiation of the shale ore (that is concentration of the kerogen before the oil-recovery step). The objective was to identify systems which could be more attractive than conventional surface retorting of ore. No experimental work was carried out. The systems analyzed consisted of beneficiation methods which could increase kerogen concentrations by at least four-fold. Potentially attractive low-enrichment methods such as density separation were not examined. The technical alternatives considered were bounded by the secondary crusher as input and raw shale oil as output.more » A sequence of ball milling, froth flotation, and retorting concentrate is not attractive for Western shales compared to conventional ore retorting; transporting the concentrate to another location for retorting reduces air emissions in the ore region but cost reduction is questionable. The high capital and energy cost s results largely from the ball milling step which is very inefficient. Major improvements in comminution seem achievable through research and such improvements, plus confirmation of other assumptions, could make high-enrichment beneficiation competitive with conventional processing. 27 figures, 23 tables.« less

14. INTERIOR OF ENGINE ROOM, CONTAINING MESTACORLISS CROSSCOMPOUND ENGINE, FOR ...

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

14. INTERIOR OF ENGINE ROOM, CONTAINING MESTA-CORLISS CROSS-COMPOUND ENGINE, FOR 40" BLOOMING MILL. THIS VIEW HIGHLIGHTS THE CRANK AND 24' DIAMETER FLYWHEEL. THE ENGINE IS A 7,940 HP MESTA-CORLISS CROSS-COMPOUND STEAM ENGINE ITS BORE AND STROKE ARE 32"X84"X60". NOTE FLY BALL GOVERNOR ON ENGINE. MILL DRIVE SHAFT ATTACHED TO PULLEY ON LOCATED ON CRANK. - Republic Iron & Steel Company, Youngstown Works, Blooming Mill & Blooming Mill Engines, North of Poland Avenue, Youngstown, Mahoning County, OH

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

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.

Synthesis of Ca(BH4)2 from Synthetic Colemanite Used in Hydrogen Storage by Mechanochemical Reaction

NASA Astrophysics Data System (ADS)

Karabulut, Ahmet F.; Guru, Metin; Boynueğri, Tuğba A.; Aydin, Mustafa Yasir

2016-08-01

In this study, synthesis of Ca(BH4)2 has been carried out with a solid phase reaction in which synthetic colemanite has been used as a raw material. Three dimensional high energy spex collider was selected for this mechanochemical reaction. Calcium borohydride is one of the most valuable metal borohydrides. In order to produce calcium borohydride economically, anhydrous colemanite mineral has been used as reactant. Calcium borohydride has been directly manufactured from anhydrous colemanite in spex-type ball milling without the need for any intermediate product. Thus, the advantages of this method over wet chemical procedure (such as having no intermediate product, no azeotropic limitations and no need of regaining product from solution after production by using evaporation, crystallization and drying processes) have made it possible to achieve the desired economical gains. Parametric experiments were conducted to determine the best conditions for the highest yield of solid phase reaction in the spex-type ball milling. Best results have been determined by using areas of related peaks in spectra of Fourier transform infrared spectroscopy (FT-IR). In order to use peaks area for determining Ca(BH4)2 concentration, a calibration graph of FT-IR absorbance peak areas has been created by using samples with known different concentrations of commercial Ca(BH4)2. Optimum amounts of calcium hydride and synthesis reaction time were found to be 2.1 times the stoichiometric ratio and 2500 min, respectively. As a result of these optimizations, the maximum yield of the solid phase reaction carried out by the spex-type ball milling has been determined as 93%.

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.

Mechanically delaminated few layered MoS2 nanosheets based high performance wire type solid-state symmetric supercapacitors

NASA Astrophysics Data System (ADS)

Krishnamoorthy, Karthikeyan; Pazhamalai, Parthiban; Veerasubramani, Ganesh Kumar; Kim, Sang Jae

2016-07-01

Two dimensional nanostructures are increasingly used as electrode materials in flexible supercapacitors for portable electronic applications. Herein, we demonstrated a ball milling approach for achieving few layered molybdenum disulfide (MoS2) via exfoliation from their bulk. Physico-chemical characterizations such as X-ray diffraction, field emission scanning electron microscope, and laser Raman analyses confirmed the occurrence of exfoliated MoS2 sheets with few layers from their bulk via ball milling process. MoS2 based wire type solid state supercapacitors (WSCs) are fabricated and examined using cyclic voltammetry (CV), electrochemical impedance spectroscopy, and galvanostatic charge discharge (CD) measurements. The presence of rectangular shaped CV curves and symmetric triangular shaped CD profiles suggested the mechanism of charge storage in MoS2 WSC is due to the formation of electrochemical double layer capacitance. The MoS2 WSC device delivered a specific capacitance of 119 μF cm-1, and energy density of 8.1 nW h cm-1 with better capacitance retention of about 89.36% over 2500 cycles, which ensures the use of the ball milled MoS2 for electrochemical energy storage devices.

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.

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.

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.

Development of CIP/graphite composite additives for electromagnetic wave absorption applications

NASA Astrophysics Data System (ADS)

Woo, Soobin; Yoo, Chan-Sei; Kim, Hwijun; Lee, Mijung; Quevedo-Lopez, Manuel; Choi, Hyunjoo

2017-09-01

In this study, the electromagnetic (EM) wave absorption ability of carbonyl iron powder (CIP)/graphite composites produced by ball milling were studied in a range of 28.5 GHz to examine the effects of the morphology and volume fraction of graphite on EM wave absorption ability. The results indicated that a ball milling technique was effective in exfoliating the graphite and covering it with CIP, thereby markedly increasing the specific surface area of the hybrid powder. The increase in the surface area and hybridization with dielectric loss materials (i.e., graphite) improved EM absorbing properties of CIP in the range of S and X bands. Specifically, the CIP/graphite composite containing 3 wt% graphite exhibited electromagnetic wave absorption of -13 dB at 7 GHz, -21 dB at 5.8 GHz, and -29 dB at 4.3 GHz after 1 h, 8 h, and 16 h of milling, respectively. [Figure not available: see fulltext.

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.

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.

Structure and magnetic properties of nanostructured MnNi alloys fabricated by mechanical alloying and annealing treatments

NASA Astrophysics Data System (ADS)

Jalal, T.; Hossein Nedjad, S.; Khalili Molan, S.

2013-05-01

A nearly equiatomic MnNi alloy was fabricated from the elemental powders by means of mechanical alloying in a planetary ball milling apparatus. X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and measurements of magnetization were conducted to identify the structural states and properties of the prepared alloys. After ball milling for 20 h, a disordered face-centered cubic (f.c.c.) solid solution was formed which increased in lattice parameter by further milling up to 50 h. An exothermic reaction took place at around 300-400°C during continuous heating of the disordered f.c.c. solid solution. This reaction is attributed to a structural ordering leading to the formation of a face-centered tetragonal (f.c.t.) phase with L10 type ordering. Examination of the magnetic properties indicated that the structural ordering increases remnant magnetization and decreases coerecivity.

Formation of Yttrium Oxysulfide Phosphor at Room Temperature

NASA Astrophysics Data System (ADS)

Shoji, Masahiko; Sakurai, Kenji

2005-12-01

Europium-doped yttrium oxysulfide (Y2O2S:Eu) phosphor was successfully synthesized at room temperature from yttrium oxide, europium oxide, and sulfur. The method employs high-energy ball milling to enable a substitution reaction between oxygen and sulfur, unlike conventional methods, such as heating in a sulfurizing atmosphere. It was found that the material is fluorescent through X-ray irradiation, and the luminescence spectra exhibit four peaks in the wavelength region from 500 to 800 nm.

Carbon/tin oxide composite electrodes for improved lithium-ion batteries

DOE PAGES

Li, Yunchao; Levine, Alan M.; Zhang, Jinshui; ...

2018-05-17

Tin and tin oxide-based electrodes are promising high-capacity anodes for lithium-ion batteries. However, poor capacity retention is the major issue with these materials due to the large volumetric expansion that occurs when lithium is alloyed with tin during lithiation and delithiation process. Here, a method to prepare a low-cost, scalable carbon and tin(II) oxide composite anode is reported. The composite material was prepared by ball milling of carbon recovered from used tire powders with 25 wt% tin(II) oxide to form lithium-ion battery anode. With the impact of energy from the ball milling, tin oxide powders were uniformly distributed inside themore » pores of waste-tire-derived carbon. During lithiation and delithiation, the carbon matrix can effectively absorb the volume expansion caused by tin, thereby minimizing pulverization and capacity fade of the electrodes. In conclusion, the as-synthesized anode yielded a capacity of 690 mAh g –1 after 300 cycles at a current density of 40 mA g –1 with a stable battery performance.« less

Carbon/tin oxide composite electrodes for improved lithium-ion batteries

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

Li, Yunchao; Levine, Alan M.; Zhang, Jinshui

Tin and tin oxide-based electrodes are promising high-capacity anodes for lithium-ion batteries. However, poor capacity retention is the major issue with these materials due to the large volumetric expansion that occurs when lithium is alloyed with tin during lithiation and delithiation process. Here, a method to prepare a low-cost, scalable carbon and tin(II) oxide composite anode is reported. The composite material was prepared by ball milling of carbon recovered from used tire powders with 25 wt% tin(II) oxide to form lithium-ion battery anode. With the impact of energy from the ball milling, tin oxide powders were uniformly distributed inside themore » pores of waste-tire-derived carbon. During lithiation and delithiation, the carbon matrix can effectively absorb the volume expansion caused by tin, thereby minimizing pulverization and capacity fade of the electrodes. In conclusion, the as-synthesized anode yielded a capacity of 690 mAh g –1 after 300 cycles at a current density of 40 mA g –1 with a stable battery performance.« less

The MillSOT-A Spiral Orbit Tribometer on a Milling Machine

NASA Technical Reports Server (NTRS)

Pepper, Stephen V.

2014-01-01

A spiral orbit tribometer (SOT) intended to characterize friction and wear phenomena has been constructed on a milling machine. The instrument, essentially a retainerless thrust bearing with one ball and flat races, is exceedingly simple and inexpensive to construct. The capabilities of the tribometer to measure both the coefficient of friction and contact electrical resistance are demonstrated with clean specimens as well as with well known lubricants such as molybdenum disulphide and Krytox oil. Operation in a purged environment of inert gas is also demonstrated. The results with these lubricants are quite close to what is obtained by other methods. Suggestions for extending the capabilities of the tribometer are given. This arrangement may find use in university mechanical engineering laboratories to introduce and study rolling contact motion as well as for research in contact mechanics and tribology.

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

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

Size Distributions and Characterization of Native and Ground Samples for Toxicology Studies

NASA Technical Reports Server (NTRS)

McKay, David S.; Cooper, Bonnie L.; Taylor, Larry A.

2010-01-01

This slide presentation shows charts and graphs that review the particle size distribution and characterization of natural and ground samples for toxicology studies. There are graphs which show the volume distribution versus the number distribution for natural occurring dust, jet mill ground dust, and ball mill ground dust.

Thermoelectric properties of (DyNiSn)1-x(DyNiSb)x composite

NASA Astrophysics Data System (ADS)

Synoradzki, Karol; Ciesielski, Kamil; Kępiński, Leszek; Kaczorowski, Dariusz

2018-05-01

High temperature thermoelectric properties of bulk and ball-milled cold-pressed (DyNiSn)1-x(DyNiSb)x composite materials have been studied. For bulk pure DyNiSn and DyNiSb samples the Seebeck coefficient reaches - 5.5 μV/K at 480 K and 120 μV/K at 540 K, respectively. Composite materials show metallic-like electrical resistivity and positive sign of Seebeck coefficient with values up to 50 times higher than in pure DyNiSn compound at 1000 K. Only for the sample with x = 0.47, the ball-milling drives to increase of Seebeck coefficient of about 37% at 650 K.

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.

DETAIL VIEW OF CLASSIFIER, TAILINGS LAUNDER TROUGH, LINE SHAFTS, AND ...

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

DETAIL VIEW OF CLASSIFIER, TAILINGS LAUNDER TROUGH, LINE SHAFTS, AND CONCENTRATION TABLES, LOOKING SOUTHWEST. SLURRY EXITING THE BALL MILL WAS COLLECTED IN AN AMALGAMATION BOX (MISSING) FROM THE END OF THE MILL, AND INTRODUCED INTO THE CLASSIFIER. THE TAILINGS LAUDER IS ON THE GROUND AT LOWER RIGHT. THE LINE SHAFTING ABOVE PROVIDED POWER TO THE CONCENTRATION TABLES BELOW AT CENTER RIGHT. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

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.

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.

A novel method for synthesizing nanoscale superionic MF-Sn2F5 (M = K, Cs) solid electrolytes

NASA Astrophysics Data System (ADS)

Podgorbunsky, Anatoly B.; Usolseva, T. I.; Sokolov, Alexander A.; Gnedenkov, S. V.; Sinebryukhov, S. L.

2017-09-01

Cesium and potassium pentafluorodistannites have been synthesized through "wet" high-energy ball milling and characterized through XRD, SEM techniques. The electrical conductivity of the systems have been investigated in the temperature range from 373 K to 513 K by means of impedance spectroscopy. It has been shown that the frequency dependent conductivity of the present system shows the power law feature. Thermally induced phase transitions has been confirmed as well as activation energy calculated from temperature variation of dc conductivity. It has been shown that synthesis in a wet medium enables one to obtain nanoparticles much smaller than in the case of "dry" milling.

Non-aqueous solution preparation of doped and undoped Li{sub x}Mn{sub y}O{sub z}

DOEpatents

Boyle, T.J.; Voigt, J.A.

1997-05-20

A method is described for generation of phase-pure doped and undoped Li{sub x}Mn{sub y}O{sub z} precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder. 1 fig.

Influence of processing on the microstructure and mechanical properties of 14YWT

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

Hoelzer, D. T.; Unocic, K. A.; Sokolov, Mikhail A.

2016-04-25

The investigation of the mechanical alloying (MA) conditions for producing the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy led to significant improvements in balancing the strength, ductility and fracture toughness properties while still maintaining the salient microstructural features consisting of ultra-fine grains and high concentration of Y-, Ti- and O-enriched nanoclusters. The implemented changes to the processing conditions included reducing the contamination of the powder during ball milling, applying a pre-extrusion annealing treatment on the ball milled powder and exploring different extrusion temperatures at 850 C (SM170 heat), 1000 C (SM185) and 1150 C (SM200). The microstructural studies ofmore » the three 14YWT heats showed similarities in the dispersion of nanoclusters and sub-micron size grains, indicating the microstructure was insensitive to the different extrusion conditions. Compared to past 14YWT heats, the three new heats showed lower strength, but higher ductility levels between 25 and 800 C and significantly higher fracture toughness values between 25 C and 700 C. The lower contamination levels of O, C and N achieved with improved ball milling conditions plus the slightly larger grain size were identified as important factors for improving the balance in mechanical properties of the three heats of 14YWT.« less

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.

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.

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

Effect of powders refinement on the tribological behavior of Ni-based composite coatings by laser cladding

NASA Astrophysics Data System (ADS)

Wang, Lingqian; Zhou, Jiansong; Yu, Youjun; Guo, Chun; Chen, Jianmin

2012-06-01

NiCr + Cr3C2 + Ag + BaF2/CaF2 composite coatings were produced on stainless steel (1Cr18Ni9Ti) substrates by laser cladding. Corresponding powders were prepared by high-energy ball milling technique. The friction and wear behavior at room temperature was investigated through sliding against the Si3N4 ball. The morphologies of the wear debris, worn surfaces of both samples and the Si3N4 ball were analyzed by scanning electron microscopy and three dimensional non-contact surface mapping. Results showed that milling time had a great effect on the size, morphology, uniformity of the powders as well as the microstructure and properties of laser cladding coatings. The wear mechanism of the coatings is dominated by abrasive wear, plastic deformation and slight adhesive wear. The consecutive evolution trend of friction coefficient, wear rate as well as microhardness of the serials of coatings produced with powders of different sizes was presented.

Effect of Surfactant Molecular Weight on Particle Morphology of SmCo5 Prepared by High Energy Ball Milling

DTIC Science & Technology

2014-04-01

nanostructured materials to the high temperatures required for surfactant removal is known to result in grain growth and oxidation . In other studies...and oxidation . In other studies, select surfactant systems, such as octanoic acid or oleylamine, have been used, however, a systematic study examining...argon atmosphere to prevent oxidation . The vial was loaded into a SPEX 8000 D mill for 1 h. After milling, each powder sample was washed with ace- tone

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.

Enhancing the corrosion resistance of the 2205 duplex stainless steel bipolar plates in PEMFCs environment by surface enriched molybdenum

NASA Astrophysics Data System (ADS)

Jinlong, Lv; Zhuqing, Wang; Tongxiang, Liang; Ken, Suzuki; Hideo, Miura

Surface molybdenum enrichment on 2205 duplex stainless steel was obtained by the ball milling technique. The electrochemical results showed molybdenum enrichment on the surface of 2205 duplex stainless steel improved its corrosion resistance in a typical proton exchange membrane fuel cell environment. This was mainly attributed to higher molybdenum content in the passive film formed on 2205 duplex stainless steel after ball milling. The decreased donor and acceptor concentrations improved significantly the corrosion resistance of surface molybdenum-enriched 2205 duplex stainless steel bipolar plates in the simulated cathodic proton exchange membrane fuel cells environment. In addition, the interfacial contact resistance of the 2205 duplex stainless steel bipolar plates slightly decreased due to surface molybdenum enrichment.

DETAIL VIEW OF LOWER TRAM TERMINAL, SECONDARY ORE BIN, CRUSHER ...

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

DETAIL VIEW OF LOWER TRAM TERMINAL, SECONDARY ORE BIN, CRUSHER FOUNDATION, AND BALL MILL FOUNDATIONS, LOOKING NORTH NORTHWEST. ORE FROM THE MINES WAS DUMPED FROM THE TRAM BUCKETS INTO THE PRIMARY ORE BIN UNDER THE TRAM TERMINAL. A SLIDING CONTROL DOOR INTRODUCED THE INTO THE JAW CRUSHER (FOUNDATIONS,CENTER). THE CRUSHED ORE WAS THEN CONVEYED INTO THE SECONDARY ORE BIN AT CENTER LEFT. A HOLE IN THE FLOOR OF THE ORE BIN PASSED ORE ONTO ANOTHER CONVEYOR THAT BROUGHT IT OUT TO THE BALL MILL(FOUNDATIONS,CENTER BOTTOM). THIS SYSTEM IS MOST LIKELY NOT THE ORIGINAL SET UP, PROBABLY INSTALLED IN THE MINE'S LAST OCCUPATION IN THE EARLY 1940s. - Keane Wonder Mine, Park Route 4 (Daylight Pass Cutoff), Death Valley Junction, Inyo County, CA

Direct catalytic production of sorbitol from waste cellulosic materials.

PubMed

Ribeiro, Lucília Sousa; Órfão, José J de Melo; Pereira, Manuel Fernando Ribeiro

2017-05-01

Cotton wool, cotton textile, tissue paper and printing paper, all potential waste cellulosic materials, were directly converted to sorbitol using a Ru/CNT catalyst in the presence of H 2 and using only water as solvent, without any acids. Conversions up to 38% were attained for the raw substrates, with sorbitol yields below 10%. Ball-milling of the materials disrupted their crystallinity, allowing reaching 100% conversion of cotton wool, cotton textile and tissue paper after 4h, with sorbitol yields around 50%. Mix-milling these materials with the catalyst greatly enhanced their conversion rate, and the materials were efficiently converted to sorbitol with a yield around 50% in 2h. However, ball- and mix-milled printing paper presented a conversion of only 50% after 5h, with sorbitol yields of 7%. Amounts of sorbitol of 0.525, 0.511 and 0.559g could be obtained from 1g of cotton wool, cotton textile and tissue paper, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effects of SiO2 nano-particles on tribological and mechanical properties of aluminum matrix composites by different dispersion methods

NASA Astrophysics Data System (ADS)

Azadi, Mahboobeh; Zolfaghari, Mehrdad; Rezanezhad, Saeid; Azadi, Mohammad

2018-05-01

This study has been presented with mechanical properties of aluminum matrix composites, reinforced by SiO2 nano-particles. The stir casting method was employed to produce various aluminum matrix composites. Different composites by varying the SiO2 nano-particle content (including 0.5 and 1 weight percents) and two dispersion methods (including ball-milling and pre-heating) were made. Then, the density, the hardness, the compression strength, the wear resistance and the microstructure of nano-composites have been studied in this research. Besides, the distribution of nano-particles in the aluminum matrix for all composites has been also evaluated by the field emission scanning electron microscopy (FESEM). Obtained results showed that the density, the elongation and the ultimate compressive strength of various nano-composites decreased by the presence of SiO2 nano-particles; however, the hardness, the wear resistance, the yield strength and the elastic modulus of composites increased by auditioning of nano-particles to the aluminum alloy. FESEM images indicated better wetting of the SiO2 reinforcement in the aluminum matrix, prepared by the pre-heating dispersion method, comparing to ball-milling. When SiO2 nano-particles were added to the aluminum alloy, the morphology of the Si phase and intermetallic phases changed, which enhanced mechanical properties. In addition, the wear mechanism plus the friction coefficient value were changed for various nano-composites with respect to the aluminum alloy.

Synthesis of Nano-Crystalline Cu-Cr Alloy by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Sheibani, S.; Heshmati-Manesh, S.; Ataie, A.

In this paper, the influence of toluene as the process control agent (PCA) and pre-milling on the extension of solid solubility of 7 wt.% Cr in Cu by mechanical alloying in a high energy ball mill was investigated. The structural evolution and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, respectively. The solid solution formation at different conditions was analyzed by copper lattice parameter change during the milling process. It was found that both the presence of PCA and pre-milling of Cr powder lead to faster dissolution of Cr. The mean crystallite size was also calculated and showed to be about 10 nm after 80 hours of milling.

Solid state amorphization in the Al-Fe binary system during high energy milling

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

Urban, P., E-mail: purban@us.es; Montes, J. M.; Cintas, J.

2013-12-16

In the present study, mechanical alloying (MA) of Al75Fe25 elemental powders mixture was carried out in argon atmosphere, using a high energy attritor ball mill. The microstructure of the milled products at different stages of milling was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The results showed that the amorphous phase content increased by increasing the milling time, and after 50 hours the amorphization process became complete. Heating the samples resulted in the crystallization of the synthesized amorphous alloys and the appearance of the equilibrium intermetallic compounds Al{sub 5}Fe{submore » 2}.« less

Half-heusler alloys with enhanced figure of merit and methods of making

DOEpatents

Ren, Zhifeng; Yan, Xiao; Joshi, Giri; Chen, Shuo; Chen, Gang; Poudel, Bed; Caylor, James Christopher

2015-06-02

Thermoelectric materials and methods of making thermoelectric materials having a nanometer mean grain size less than 1 micron. The method includes combining and arc melting constituent elements of the thermoelectric material to form a liquid alloy of the thermoelectric material and casting the liquid alloy of the thermoelectric material to form a solid casting of the thermoelectric material. The method also includes ball milling the solid casting of the thermoelectric material into nanometer mean size particles and sintering the nanometer size particles to form the thermoelectric material having nanometer scale mean grain size.

Preparation of Cu2ZnSnS4 nano-crystalline powder by mechano-chemical method

NASA Astrophysics Data System (ADS)

Alirezazadeh, Farzaneh; Sheibani, Saeed; Rashchi, Fereshteh

2018-01-01

Copper zinc tin sulfide (Cu2ZnSnS4, CZTS) is one of the most promising ceramic materials as an absorber layer in solar cells due to its suitable band gap, high absorption coefficient and non-toxic and environmental friendly constituent elements. In this work, nano-crystalline CZTS powder was synthesized by mechanical milling. Elemental powders of Cu, Zn, Sn and were mixed in atomic ratio of 2:1:1:4 according to the stoichiometry of Cu2ZnSnS4 and then milled in a planetary high energy ball mill under argon atmosphere. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and diffusion reflectance spectroscopy (DRS). XRD results confirm the formation of single-phase CZTS with kesterite structure after 20 h of milling. Also, the mean crystallite size was about 35 nm. SEM results show that after 20 h of milling, the product has a relatively uniform particle size distribution. Optical properties of the product indicate that the band gap of prepared CZTS is 1.6 eV which is near to the optimum value for photovoltaic solar cells showing as a light absorber material in solar energy applications.

Properties and rapid low-temperature consolidation of nanocrystalline Fe-ZrO2 composite by pulsed current activated sintering

NASA Astrophysics Data System (ADS)

Kang, Hyun-Su; Ko, In-Yong; Yoon, Jin-Kook; Doh, Jung-Mann; Hong, Kyung-Tae; Shon, In-Jin

2011-02-01

Nanopowders of Fe and ZrO2 were synthesized from Fe2O3 and Zr by high-energy ball milling. The powder sizes of Fe and ZrO2 were 70 nm and 12 nm, respectively. Highly dense nanostructured 4/3Fe-ZrO2 composite was consolidated by a pulsed current activated sintering method within 1 minute from the mechanically synthesized powders (Fe-ZrO2) and horizontal milled Fe2O3+Zr powders under the 1 GPa pressure. The grain sizes of Fe and ZrO2 in the composite were calculated. The average hardness and fracture toughness values of nanostuctured 4/3Fe-ZrO2 composite were investigated.

Split-ball resonator as a three-dimensional analogue of planar split-rings

NASA Astrophysics Data System (ADS)

Kuznetsov, Arseniy I.; Miroshnichenko, Andrey E.; Hsing Fu, Yuan; Viswanathan, Vignesh; Rahmani, Mohsen; Valuckas, Vytautas; Ying Pan, Zhen; Kivshar, Yuri; Pickard, Daniel S.; Luk'Yanchuk, Boris

2014-01-01

Split-ring resonators are basic elements of metamaterials, which can induce a magnetic response in metallic nanosctructures. Tunability of such response up to the visible frequency range is still a challenge. Here we introduce the concept of the split-ball resonator and demonstrate the strong magnetic response in the visible for both gold and silver spherical plasmonic nanoparticles with nanometre scale cuts. We realize this concept experimentally by employing the laser-induced transfer method to produce near-perfect metallic spheres and helium ion beam milling to make cuts with the clean straight sidewalls and nanometre resolution. The magnetic resonance is observed at 600 nm in gold and at 565 nm in silver nanoparticles. This method can be applied to the structuring of arbitrary three-dimensional features on the surface of nanoscale resonators. It provides new ways for engineering hybrid resonant modes and ultra-high near-field enhancement.

Effect of milling on DSC thermogram of excipient adipic acid.

PubMed

Ng, Wai Kiong; Kwek, Jin Wang; Yuen, Aaron; Tan, Chin Lee; Tan, Reginald

2010-03-01

The purpose of this research was to investigate why and how mechanical milling results in an unexpected shift in differential scanning calorimetry (DSC) measured fusion enthalpy (Delta(fus)H) and melting point (T(m)) of adipic acid, a pharmaceutical excipient. Hyper differential scanning calorimetry (hyper-DSC) was used to characterize adipic acid before and after ball-milling. An experimental study was conducted to evaluate previous postulations such as electrostatic charging using the Faraday cage method, crystallinity loss using powder X-ray diffraction (PXRD), thermal annealing using DSC, impurities removal using thermal gravimetric analysis (TGA) and Karl Fischer titration. DSC thermograms showed that after milling, the values of Delta(fus)H and T(m) were increased by approximately 9% and 5 K, respectively. Previous suggestions of increased electrostatic attraction, change in particle size distribution, and thermal annealing during measurements did not explain the differences. Instead, theoretical analysis and experimental findings suggested that the residual solvent (water) plays a key role. Water entrapped as inclusions inside adipic acid during solution crystallization was partially evaporated by localized heating at the cleaved surfaces during milling. The correlation between the removal of water and melting properties measured was shown via drying and crystallization experiments. These findings show that milling can reduce residual solvent content and causes a shift in DSC results.

Influence of processing on the microstructure and mechanical properties of 14YWT

DOE PAGES

Hoelzer, David T.; Unocic, Kinga A.; Sokolov, Mikhail A.; ...

2015-12-15

In this study, the investigation of the mechanical alloying (MA) conditions for producing the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy led to significant improvements in balancing the strength, ductility and fracture toughness properties while still maintaining the salient microstructural features consisting of ultra-fine grains and high concentration of Y-, Ti- and O-enriched nanoclusters. The implemented changes to the processing conditions included reducing the contamination of the powder during ball milling, applying a pre-extrusion annealing treatment on the ball milled powder and exploring different extrusion temperatures at 850 °C (SM170 heat), 1000 °C (SM185) and 1150 °C (SM200). Themore » microstructural studies of the three 14YWT heats showed similarities in the dispersion of nanoclusters and sub-micron size grains, indicating the microstructure was insensitive to the different extrusion conditions. Compared to past 14YWT heats, the three new heats showed lower strength, but higher ductility levels between 25 and 800 °C and significantly higher fracture toughness values between 25 °C and 700 °C. The lower contamination levels of O, C and N achieved with improved ball milling conditions plus the slightly larger grain size were identified as important factors for improving the balance in mechanical properties of the three heats of 14YWT.« less

Solid-state characterization and dissolution properties of meloxicam-moringa coagulant-PVP ternary solid dispersions.

PubMed

Noolkar, Suhail B; Jadhav, Namdeo R; Bhende, Santosh A; Killedar, Suresh G

2013-06-01

The effect of ternary solid dispersions of poor water-soluble NSAID meloxicam with moringa coagulant (obtained by salt extraction of moringa seeds) and polyvinylpyrrolidone on the in vitro dissolution properties has been investigated. Binary (meloxicam-moringa and meloxicam-polyvinylpyrrolidone (PVP)) and ternary (meloxicam-moringa-PVP) systems were prepared by physical kneading and ball milling and characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, and X-ray diffractometry. The in vitro dissolution behavior of meloxicam from the different products was evaluated by means of United States Pharmacopeia type II dissolution apparatus. The results of solid-state studies indicated the presence of strong interactions between meloxicam, moringa, and PVP which were of totally amorphous nature. All ternary combinations were significantly more effective than the corresponding binary systems in improving the dissolution rate of meloxicam. The best performance in this respect was given by the ternary combination employing meloxicam-moringa-PVP ratio of [1:(3:1)] prepared by ball milling, with about six times increase in percent dissolution rate, whereas meloxicam-moringa (1:3) and meloxicam-PVP (1:4) prepared by ball milling improved dissolution of meloxicam by almost 3- and 2.5-folds, respectively. The achieved excellent dissolution enhancement of meloxicam in the ternary systems was attributed to the combined effects of impartation of hydrophilic characteristic by PVP, as well as to the synergistic interaction between moringa and PVP.

Extending the solvent-free MALDI sample preparation method.

PubMed

Hanton, Scott D; Parees, David M

2005-01-01

Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.

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

Development of a nanosuspension for iv administration: From miniscale screening to a freeze dried formulation.

PubMed

Frank, Kerstin J; Boeck, Georg

2016-05-25

The aim was to develop a nanosuspension of the poorly soluble BI XX. The nanosuspension is intended for intravenous (iv) administration in preclinical studies and should not cause any unwanted side effects. Thus, only stabilizers that are accepted for iv application should be used and isotonicity, euhydria and the absence of living microorganisms were targeted. Suspensions were prepared in a ball-mill (mixing mill MM 400 from Retsch). There were various vials used as containers; HPLC-vials were used for the small scale screening of stabilizers and injection vials for preparation of larger quantities of the nanosuspensions. Particle size distribution was analyzed by laser diffraction measurement (Mastersizer 2000). Lyophilization was used for processing of the suspensions (Christ freeze dryer). Stable nanosuspensions (d90 remained <1μm up to 7days) were prepared with several FDA-accepted stabilizers. Freeze drying was evaluated for one formulation containing 2% of the API, 0.5% of arginine and 4% of mannitol. The particle size distribution before freeze drying and after re-dispersion was comparable. After milling for 2h, no living microorganisms were detected in the nanosuspension. Various FDA accepted excipients were identified which resulted in stable nanosuspensions of BI XX. The most stable formulation was successfully freeze dried. It was proven that milling in the ball-mill decreases the presence of living microorganisms. Copyright © 2016. Published by Elsevier B.V.

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.

Reactive Fusion Welding for Ultra-High Temperature Ceramic Composite Joining

DTIC Science & Technology

2015-03-16

Titanium diboride TiC-Titanium carbide C-Carbon SiC - Silicon carbide B4C-Boron carbide 67 W-Tungsten WC-Tungsten carbide ZrB2-20ZrC-ZrB2...ceramics with a nominal carbide content of 20 vol% were prepared. Starting powders were mechanically mixed by ball milling ZrB2 (H.C. Starck; Grade B...0.50 wt%, or ~1.5 vol%. Milling was carried out in acetone for 2 hours using tungsten carbide media. After milling, the powder slurry was dried

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.

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

Shock-induced reaction synthesis of cubic boron nitride

NASA Astrophysics Data System (ADS)

Beason, M. T.; Pauls, J. M.; Gunduz, I. E.; Rouvimov, S.; Manukyan, K. V.; Matouš, K.; Son, S. F.; Mukasyan, A.

2018-04-01

Here, we report ultra-fast (0.1-5 μs) shock-induced reactions in the 3B-TiN system, leading to the direct synthesis of cubic boron nitride, which is extremely rare in nature and is the second hardest material known. Composite powders were produced through high-energy ball milling to provide intimate mixing and subsequently shocked using an explosive charge. High-resolution transmission electron microscopy and X-ray diffraction confirm the formation of nanocrystalline grains of c-BN produced during the metathetical reaction between boron and titanium nitride. Our results illustrate the possibility of rapid reactions enabled by high-energy ball milling possibly occurring in the solid state on incredibly short timescales. This process may provide a route for the discovery and fabrication of advanced compounds.

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.

Near-neighbor mixing and bond dilation in mechanically alloyed Cu-Fe

NASA Astrophysics Data System (ADS)

Harris, V. G.; Kemner, K. M.; Das, B. N.; Koon, N. C.; Ehrlich, A. E.; Kirkland, J. P.; Woicik, J. C.; Crespo, P.; Hernando, A.; Garcia Escorial, A.

1996-09-01

Extended x-ray-absorption fine-structure (EXAFS) measurements were used to obtain element-specific, structural, and chemical information of the local environments around Cu and Fe atoms in high-energy ball-milled CuxFe1-x samples (x=0.50 and 0.70). Analysis of the EXAFS data shows both Fe and Cu atoms reside in face-centered-cubic sites where the first coordination sphere consists of a mixture of Fe and Cu atoms in a ratio which reflects the as-prepared stoichiometry. The measured bond distances indicate a dilation in the bonds between unlike neighbors which accounts for the lattice expansion measured by x-ray diffraction. These results indicate that metastable alloys having a positive heat of mixing can be prepared via the high-energy ball-milling process.

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.

High-Energy Ball Milling as Green Process To Vitrify Tadalafil and Improve Bioavailability.

PubMed

Krupa, Anna; Descamps, Marc; Willart, Jean-François; Strach, Beata; Wyska, Elżbieta; Jachowicz, Renata; Danède, Florence

2016-11-07

In this study, the suitability of high-energy ball milling was investigated with the aim to vitrify tadalafil (TD) and improve its bioavailability. To achieve this goal, pure TD as well as binary mixtures composed of the drug and Soluplus (SL) were coprocessed by high-energy ball milling. Modulated differential scanning calorimetry (MDSC) and X-ray powder diffraction (XRD) demonstrated that after such coprocessing, the crystalline form of TD was transformed into an amorphous form. The presence of a single glass transition (T g ) for all the comilled formulations indicated that TD was dispersed into SL at the molecular level, forming amorphous molecular alloys, regardless of the drug concentration. The high values of T g determined for amorphous formulations, ranging from 70 to 147 °C, foreshow their high stability during storage at room temperature, which was verified by XRD and MDSC studies. The stabilizing effect of SL on the amorphous form of TD in comilled formulations was confirmed. Dissolution tests showed immediate drug release with sustained supersaturation in either simulated gastric fluid of pH 1.2 or in phosphate buffer of pH 7.2. The beneficial effect of both amorphization and coamorphization on the bioavailability of TD was found. In comparison to aqueous suspension, the relative bioavailability of TD was only 11% for its crystalline form and 53% for the crystalline physical mixture, whereas the bioavailability of milled amorphous TD and the comilled solid dispersion was 128% and 289%, respectively. Thus, the results provide evidence that not only the presence of polymeric surfactant but also the vitrification of TD is necessary to improve bioavailability.

Laser ablation ICP-MS analysis on nano-powder pellets and applications to granite bulk rock analysis

NASA Astrophysics Data System (ADS)

Wu, Shitou; Karius, Volker; Wörner, Gerhard

2017-04-01

Granites are a ubiquitous component of the continental crust and knowing their precise trace element signatures is essential in understanding the origins and evolution of the continental crust. ICP-MS bulk analysis of granite is generally conducted on solution after acid-digestion. However this technique has several deficiencies related to the difficulty of completely dissolving accessary minerals such as zircon and the instability/adsorption of high valence trace elements (Nb, Ta et al.) in acid solutions. The development of a nano-powder pellet technique by using wet milling procedure, and its combination with laser ablation ICP-MS has been proposed to overcome these problems. In this study, we produced nano-powders from a series of granite rock standards by wet milling in agate using a high power planetary ball mill instrument. The procedure was tested and optimized by modifying parameters (ball to powder ratio, water to powder ratio, milling power etc.). Characterization of nano-powders was conducted by various techniques including electron microprobe (EMP), secondary electron imaging, polarizing microscope, and laser particle size analyzer (LPSA) and laser scanning confocal microscope (LSCM). Particle sizes range from a few nm to 5 μm with a small secondary mode at around 10 to 20 μm that probably represent particle aggregates rather than remaining crystal grains after milling. Pellets of 5 mm in diameter were pressed into molds of cellulose at 1.75 *103 N/cm2. Surface roughness of the pellets was measured by LSCM and gave a Ra of 0.494 μm, which is an order higher than the surface of polished ATGH-G reference glass surface (Ra: 0.048 μm), but sufficient for laser ablation. Sources of contamination either from abrading agate balls or from ultrapure water were evaluated and quantified. The homogeneity of powder pellets down to less than 5 μm size was documented based on EMPA element mapping and statistical analyses of LA-ICP-MS in discrete spot and line scanning analytical mode. We report data from major to trace element (to < 0.1 ppm) of currently available international granite reference materials (JG-2, JG-3, GWB07103, GEB07111, GSP-2 and G-3) to evaluate analytical precision and accuracy of LA-ICP-MS measurements. Our results illustrate the potential of this method for high precision analysis of trace elements and e.g. Zr/Hf and Nb/Ta ratios in granites.

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

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.

Graphite-to-Graphene: Total Conversion.

PubMed

Buzaglo, Matat; Bar, Ilan Pri; Varenik, Maxim; Shunak, Liran; Pevzner, Svetlana; Regev, Oren

2017-02-01

The rush to develop graphene applications mandates mass production of graphene sheets. However, the currently available complex and expensive production technologies are limiting the graphene commercialization. The addition of a protective diluent to graphite during ball-milling is demonstrated to result in a game-changer yield (>90%) of defect-free graphene, whose size is controlled by the milling energy and the diluent type. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigating the reactivity of pMDI with wood cell walls using high-resolution solution-state NMR spectroscopy

Treesearch

Daniel J. Yelle; John Ralph; Charles R. Frihart

2009-01-01

The objectives of this study are the following: (1) Use solution-state NMR to assign contours in HSQC spectra of the reaction products between pMDI model compounds and: (a) lignin model compounds, (b) milled-wood lignin, (c) ball-milled wood, (d) microtomed loblolly pine; (2) Determine where and to what degree urethane formation occurs with loblolly pine cell wall...

Impact Ignition of Low Density Mechanically Activated and Multilayer Foil Ni/Al

NASA Astrophysics Data System (ADS)

Beason, Matthew; Mason, B.; Son, Steven; Groven, Lori

2013-06-01

Mechanical activation (MA) via milling of reactive materials provides a means of lowering the ignition threshold of shock initiated reactions. This treatment provides a finely mixed microstructure with wide variation in the resulting scales of the intraparticle microstructure that makes model validation difficult. In this work we consider nanofoils produced through vapor deposition with well defined periodicity and a similar degree of fine scale mixing. This allows experiments that may be easier to compare with computational models. To achieve this, both equimolar Ni/Al powder that has undergone MA using high energy ball milling and nanofoils milled into a powder using low energy ball milling were used. The Asay Shear impact experiment was conducted on both MA Ni/Al and Ni/Al nanofoil-based powders at low densities (<60%) to examine their impact response and reaction behavior. Scanning electron microscopy and energy-dispersive x-ray spectroscopy were used to verify the microstructure of the materials. The materials' mechanical properties were evaluated using nano-indentation. Onset temperatures were evaluated using differential thermal analysis/differential scanning calorimetry. Impact ignition thresholds, burning rates, temperature field, and ignition delays are 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.

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.

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.

Development of Oxide Dispersion Strengthened MCrAlY Coatings

NASA Astrophysics Data System (ADS)

Bobzin, K.; Schläfer, T.; Richardt, K.; Brühl, M.

2008-12-01

MCrAlY materials are widely used as bond coats for thermal barrier coatings on turbine blades. The aim of this work is to improve mechanical properties and wear resistance of thermal sprayed NiCoCrAlY-coatings by strengthening the coating with hard phase particles. In order to retain the effect of the dispersion reinforcement at high temperatures, the use of temperature-stable oxide hard phases such as ZrO2-Y2O3 is necessary. To realize this new material structure, the high-energy ball-milling process is applied and analyzed. The mixture ratio between NiCoCrAlY and ZrO2-Y2O3 was varied between 5 and 10 wt.% ZrO2-Y2O3. The influences of the milling time of the high-energy ball-milling process on the distribution of the hard phases in the metal matrix were analyzed. After spraying with a HVOF system the mechanical properties of the coatings are measured and compared with conventional NiCoCrAlY coatings.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

Phase composition and microstructure of WC-Co alloys obtained by selective laser melting

NASA Astrophysics Data System (ADS)

Khmyrov, Roman S.; Shevchukov, Alexandr P.; Gusarov, Andrey V.; Tarasova, Tatyana V.

2018-03-01

Phase composition and microstructure of initial WC, BK8 (powder alloy 92 wt.% WC-8 wt.% Co), Co powders, ball-milled powders with four different compositions (1) 25 wt.% WC-75 wt.% Co, (2) 30 wt.% BK8-70 wt.% Co, (3) 50 wt.% WC-50 wt.% Co, (4) 94 wt.% WC-6 wt.% Co, and bulk alloys obtained by selective laser melting (SLM) from as-milled powders in as-melted state and after heat treatment were investigated by scanning electron microscopy and X-ray diffraction analysis. Initial and ball-milled powders consist of WC, hexagonal α-Co and face-centered cubic β-Co. The SLM leads to the formation of major new phases W3Co3C, W4Co2C and face-centered cubic β-Co-based solid solution. During the heat treatment, there occurs partial decomposition of the face-centered cubic β-Co-based solid solution with the formation of W2C and hexagonal α-Co solid solution. The microstructure of obtained bulk samples, in general, corresponds to the observed phase composition.

High-speed vibration-milling-promoted synthesis of symmetrical frameworks containing two or three pyrrole units

PubMed Central

Leonardi, Marco; Villacampa, Mercedes

2017-01-01

The pseudo-five-component reaction between β-dicarbonyl compounds (2 molecules), diamines and α-iodoketones (2 molecules), prepared in situ from aryl ketones, was performed efficiently under mechanochemical conditions involving high-speed vibration milling with a single zirconium oxide ball. This reaction afforded symmetrical frameworks containing two pyrrole or fused pyrrole units joined by a spacer, which are of interest in the exploration of chemical space for drug discovery purposes. The method was also extended to the synthesis of one compound containing three identical pyrrole fragments via a pseudo-seven-component reaction. Access to compounds having a double bond in their spacer chain was achieved by a different approach involving the homodimerization of 1-allyl- or 1-homoallylpyrroles by application of cross-metathesis chemistry. PMID:29062414

Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

PubMed

Balamurugan, S; Melba, K

2015-06-01

The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.

Investigation of room temperature ferromagnetic nanoparticles of Gd 5Si 4

DOE PAGES

Hadimani, R. L.; Gupta, S.; Harstad, S. M.; ...

2015-07-06

Gd 5(Si xGe 1-x) 4 compounds undergo first-order phase transitions close to room temperature when x ~ = 0.5, which are accompanied by extreme changes of properties. We report the fabrication of the nanoparticles of one of the parent compounds-Gd 5Si 4-using high-energy ball milling. Crystal structure, microstructure, and magnetic properties have been investigated. Particles agglomerate at long milling times, and the particles that are milled >20 min lose crystallinity and no longer undergo magnetic phase transition close to 340 K, which is present in a bulk material. The samples milled for >20 min exhibit a slightly increased coercivity. Asmore » a result, magnetization at a high temperature of 275K decreases with the increase in the milling time.« less

Mechanochemistry-assisted synthesis of hierarchical porous carbons applied as supercapacitors

PubMed Central

Leistenschneider, Desirée; Jäckel, Nicolas; Hippauf, Felix; Presser, Volker

2017-01-01

A solvent-free synthesis of hierarchical porous carbons is conducted by a facile and fast mechanochemical reaction in a ball mill. By means of a mechanochemical ball-milling approach, we obtained titanium(IV) citrate-based polymers, which have been processed via high temperature chlorine treatment to hierarchical porous carbons with a high specific surface area of up to 1814 m2 g−1 and well-defined pore structures. The carbons are applied as electrode materials in electric double-layer capacitors showing high specific capacitances with 98 F g−1 in organic and 138 F g−1 in an ionic liquid electrolyte as well as good rate capabilities, maintaining 87% of the initial capacitance with 1 M TEA-BF4 in acetonitrile (ACN) and 81% at 10 A g−1 in EMIM-BF4. PMID:28781699

Filtration effects on ball bearing life and condition in a contaminated lubricant

NASA Technical Reports Server (NTRS)

Loewenthal, S. H.; Moyer, D. W.

1978-01-01

Ball bearings were fatigue tested with a noncontaminated MIL-L-23699 lubricant and with a contaminated MIL-L-23699 lubricant under four levels of filtration. The test filters had absolute particle removal ratings of 3, 30, 49, and 105 microns. Aircraft turbine engine contaminants were injected into the filter's supply line at a constant rate of 125 milligrams per bearing hour. Bearing life and running track condition generally improved with finer filtration. The experimental lives of 3- and 30-micron filter bearings were statistically equivalent, approaching those obtained with the noncontaminated lubricant bearings. Compared to these bearings, the lives of the 49-micron bearings were statistically lower. The 105-micron bearings experienced gross wear. The degree of surface distress, weight loss, and probable failure mode were dependent on filtration level, with finer filtration being clearly beneficial.

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.

Enhancement of exchange coupling interaction of NdFeB/MnBi hybrid magnets

NASA Astrophysics Data System (ADS)

Nguyen, Truong Xuan; Nguyen, Khanh Van; Nguyen, Vuong Van

2018-03-01

MnBi ribbons were fabricated by melt - spinning with subsequent annealing. The MnBi ribbons were ground and mixed with NdFeB commercial Magnequench powders (MQA). The hybrid powder mixtures were subjected thrice to the annealing and ball-milling route. The hybrid magnets (100 - x)NdFeB/xMnBi, x=0, 30, 40, 50 and 100 wt% were in-mold aligned in an 18 kOe magnetic field and warm compacted at 290 °C by 2000 psi uniaxial pressure for 10 min. An enhancement of the exchange coupling of NdFeB/MnBi hybrid magnets was obtained by optimizing the magnets' microstructures via annealing and ball-milling processes. The magnetic properties of prepared NdFeB/MnBi hybrid magnets were studied and discussed in details.

Microstructure and magnetic behavior of Cu-Co-Si ternary alloy synthesized by mechanical alloying and isothermal annealing

NASA Astrophysics Data System (ADS)

Chabri, Sumit; Bera, S.; Mondal, B. N.; Basumallick, A.; Chattopadhyay, P. P.

2017-03-01

Microstructure and magnetic behavior of nanocrystalline 50Cu-40Co-10Si (at%) alloy prepared by mechanical alloying and subsequent isothermal annealing in the temperature range of 450-650 °C have been studied. Phase evolution during mechanical alloying and isothermal annealing is characterized by X-ray diffraction (XRD), differential thermal analyzer (DTA), high resolution transmission electron microscopy (HRTEM) and magnetic measurement. Addition of Si has been found to facilitate the metastable alloying of Co in Cu resulting into the formation of single phase solid solution having average grain size of 9 nm after ball milling for 50 h duration. Annealing of the ball milled alloy improves the magnetic properties significantly and best combination of magnetic properties has been obtained after annealing at 550 °C for 1 h duration.

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.

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.

Flue gas desulfurization chemistry studies: limestone grindability. Volume 2. Grindability testing. Final report

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

Richmann, D.L.; Luke, K.W.; Terry, J.C.

1984-07-01

The results of a study to determine the relative grindability of US limestones and to relate grindability to petrographic properties are presented in this report. A laboratory ball mill test was developed to provide a quick and simple measure of grindability. These values were then used to explore possible correlations between grindability and the chemical and physical properties of the limestones. Chemical analyses and thin section petrographic analyses were used to characterize the limestone samples. The results of the laboratory ball mill test were compared to the results of an industrial grinding test, the Bond Work Index, for six samplesmore » which covered the grindability range. The two tests compared well with a correlation coefficient greater than 0.9. While the laboratory test is not sufficient to provide ball mill design specifications, it can be used as a screening and quality control test. The grinding results, expressed as a grindability index, ranged in values from 2 to 15. This represents a seven-fold range in the relative difficulties to grind for the limestones tested. From the petrographic analysis results, a strong correlation was found between the grindability and the fraction of macrocrystalline (> 5 ..mu..m) carbonate minerals present in the limestone. However, based on the high degree of variability characteristic of most limestone deposits, petrographic information should, in general, only be used to qualitatively predict the grindability of a specific limestone. An actual grinding test is recommended for a quantitative evaluation.« 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.

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.

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.

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.

Structural transformation in nano-structured CuAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} system

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

Mehta, D. K., E-mail: daxabjoshi@gmail.com; Chhantbar, M. C.; Joshi, H. H.

Polycrystalline spinel ferrite system CuAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} (x=0.2, 0.6) was synthesized by solid-state reaction route. Nanoparticles of the samples have been prepared by using high energy ball milling technique with different milling durations and characterized by X-ray Diffraction and Tunneling Electron Microscope. It is observed that the structural transformation occurred from Cubic to tetragonal and particle size varied between 29 nm -14 nm with increase of milling time.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

Yepes, N.; Orozco, J.; Caamaño, Z.; Mass, J.; Pérez, G.

2014-04-01

Nanostructured Fe50Co50 alloy was prepared by mechanical alloying of Fe and Co powders in a planetary high energy ball milling. The microstructure and structural evolution of the alloy have been investigated as a function of milling time (0 h, 8 h, 20 h and 35 h) by scanning electron microscopy (SEM) and X-Ray diffraction (XRD) characterization techniques. SEM micrographs showed different powder particles morphologies during the mechanical alloying stages. By XRD analysis it could be identified the structural phases of the alloy and the crystallite size was calculated as a function of the milling time.

Fabrication and characterization of crushed titanium-beryllium intermetallic compounds

NASA Astrophysics Data System (ADS)

Kim, Jae-Hwan; Nakamichi, Masaru

2018-01-01

To develop a technique for the mass production of beryllide pebbles, a crushing method for the granulation of beryllides was used in this study. Two types of crushed Be12Ti pebbles were prepared using mortar-ground (MG) and planetary-ball-milled (PM) powders. A granulation yield of approximately 50 wt.% with sizes in the range of 0.85-1.18 mm was achieved. Scanning electron microscopy (SEM) images revealed that the MG pebbles exhibited larger porosity because the larger size of the powder resulted in lower density with higher porosity. However, the considerably larger fraction of fine pores in the PM pebbles resulted in an increased Brunauer-Emmett-Teller (BET) specific surface area, as clearly demonstrated by high-magnification SEM images. To evaluate the reactivity with water vapor, the weight gain and H2 generation rate were also investigated. The results suggested that the PM pebbles exhibited notably lower reactivity, weight gain, and H2 generation rate, which may be due to the dramatically decreased BET specific surface. The fine pores were filled with stable oxides followed by a significant decrease of the surface area during oxidation. Optimization was performed to improve the circularity of the crushed pebbles. Grinding tests using planetary milling without balls for different times clearly demonstrated that the circularity improved (with an estimated value of 0.8) by cutting and polishing the sharp edges; however, long-duration milling for 99 h resulted in attachment of the polished powders to the pebble surface, leading to surface color variation of the crushed pebbles.

Influence of platinum group metal-free catalyst synthesis on microbial fuel cell performance

NASA Astrophysics Data System (ADS)

Santoro, Carlo; Rojas-Carbonell, Santiago; Awais, Roxanne; Gokhale, Rohan; Kodali, Mounika; Serov, Alexey; Artyushkova, Kateryna; Atanassov, Plamen

2018-01-01

Platinum group metal-free (PGM-free) ORR catalysts from the Fe-N-C family were synthesized using sacrificial support method (SSM) technique. Six experimental steps were used during the synthesis: 1) mixing the precursor, the metal salt, and the silica template; 2) first pyrolysis in hydrogen rich atmosphere; 3) ball milling; 4) etching the silica template using harsh acids environment; 5) the second pyrolysis in ammonia rich atmosphere; 6) final ball milling. Three independent batches were fabricated following the same procedure. The effect of each synthetic parameters on the surface chemistry and the electrocatalytic performance in neutral media was studied. Rotating ring disk electrode (RRDE) experiment showed an increase in half wave potential and limiting current after the pyrolysis steps. The additional improvement was observed after etching and performing the second pyrolysis. A similar trend was seen in microbial fuel cells (MFCs), in which the power output increased from 167 ± 2 μW cm-2 to 214 ± 5 μW cm-2. X-ray Photoelectron Spectroscopy (XPS) was used to evaluate surface chemistry of catalysts obtained after each synthetic step. The changes in chemical composition were directly correlated with the improvements in performance. We report outstanding reproducibility in both composition and performance among the three different batches.

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

In vitro bond strength and fatigue stress test evaluation of different adhesive cements used for fixed space maintainer cementation

PubMed Central

Cantekin, Kenan; Delikan, Ebru; Cetin, Secil

2014-01-01

Objective: The purposes of this research were to (1) compare the shear-peel bond strength (SPBS) of a band of a fixed space maintainer (SM) cemented with five different adhesive cements; and (2) compare the survival time of bands of SM with each cement type after simulating mechanical fatigue stress. Materials and Methods: Seventy-five teeth were used to assess retentive strength and another 50 teeth were used to assess the fatigue survival time. SPBS was determined with a universal testing machine. Fatigue testing was conducted in a ball mill device. Results: The mean survival time of bands cemented with R & D series Nova Glass-LC (6.2 h), Transbond Plus (6.7 h), and R & D series Nova Resin (6.8 h) was significantly longer than for bands cemented with Ketac-Cem (5.4 h) and GC Equia (5.2 h) (P < 0.05). Conclusion: Although traditional glass ionomer cement (GIC) cement presented higher retentive strength than resin-based cements (resin, resin modified GIC, and compomer cement), resin based cements, especially dual cure resin cement (nova resin cement) and compomer (Transbond Plus), can be expected to have lower failure rates for band cementation than GIC (Ketac-Cem) in the light of the results of the ball mill test. PMID:25202209

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.

Preparation and characterization of natural bentonite in to nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Sirait, Makmur; Bukit, Nurdin; Siregar, Nurdin

2017-01-01

The nanoparticle based on natural bentonite from Pahae village had been prepared using co-precipitation method. Bentonite was dried in the oven at 100°C during a week. Bentonite is crushed using a mortal and milled by planetary ball mill to obtain the powder form. Further, the bentonite powder is activated with chemical reaction by dissolves the 50 g bentonite to 100 ml of HCl at 10 M. The magnetic stirrer was employed to mix the solution at 300 rpm and temperature 70°C. After that, the bentonite solution is washed using distilled water until the pH is neutral. The bentonite powder is calcined at temperature of 600°C for 1 hour with fix increment 150°C. Finally, the powder is given High Energy Milling (HEM) treatment for 30 minutes to obtain the particle size. The X-ray Difractometer (XRD) and Scanning Electron Microscope (SEM) were used to characterize. From the characterization results it is reported that the average of bentonite nanoparticle size is 35.26 nm and the chemical constituents of natural bentonite Pahae are Al, Si, Ca, Fe and Ti.

The kinetics of composite particle formation during mechanical alloying

NASA Technical Reports Server (NTRS)

Aikin, B. J. M.; Courtney, T. H.

1993-01-01

The kinetics of composite particle formation during attritor milling of insoluble binary elemental powders have been examined. The effects of processing conditions (i.e., mill power, temperature, and charge ratio) on these kinetics were studied. Particle size distributions and fractions of elemental and composite particles were determined as functions of milling time and processing conditions. This allowed the deduction of phenomenological rate constants describing the propensity for fracture and welding during processing. For the mill-operating conditions investigated, the number of particles in the mill generally decreased with milling time, indicating a greater tendency for particle welding than fracture. Moreover, a bimodal size distribution is often obtained as a result of preferential welding. Copper and chromium 'alloy' primarily by encapsulation of Cr particles within Cu. This form of alloying also occurs in Cu-Nb alloys processed at low mill power and/or for short milling times. For other conditions, however, Cu-Nb alloys develop a lamellar morphology characteristic of mechanically alloyed two-phase ductile metals. Increasing mill power or charge (ball-to-powder weight) ratio (CR) increases the rate of composite particle formation.

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

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.

Magnetic behavior of the nanophase of YbNi2 alloys

NASA Astrophysics Data System (ADS)

Ivanshin, V. A.; Gataullin, E. M.; Sukhanov, A. A.; Ivanshin, N. A.; Rojas, D. P.; Fernández Barquín, L.

2017-04-01

Variations in magnetic properties of the heavy-fermion YbNi2 alloy when milled in a high energy ball milling system have been investigated. The ferromagnetic transition ( T C = 10.4 K) in the initial sample almost vanishes after milling, which leads to the appearance of a magnetic transition at T* = 3.2 K in nanocrystallites. Before milling, processes of spin-lattice relaxation of the Orbach-Aminov type with the participation of the first excited Stark sublevel of the Yb3+ ion located at 75 K are dominating in the electron spin dynamics in the paramagnetic phase of the alloy. A comparative study of the temperature dependence of the magnetic properties and spectra of electron paramagnetic resonance in poly- and nanocrystalline samples indicates the existence of a magnetic inhomogeneity of the compound arising upon milling.

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.

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.

Energy transfer and kinetics in mechanochemistry.

PubMed

Chen, Zhiliang; Lu, Shengyong; Mao, Qiongjing; Buekens, Alfons; Wang, Yuting; Yan, Jianhua

2017-11-01

Mechanochemistry (MC) exerts extraordinary degradation and decomposition effects on many chlorinated, brominated, and even fluorinated persistent organic pollutants (POPs). However, its application is still limited by inadequate study of its reaction kinetic aspects. In the present work, the ball motion and energy transfer in planetary ball mill are investigated in some detail. Almost all milling parameters are summarised in a single factor-total effective impact energy. Furthermore, the MC kinetic between calcium oxide/Al and hexachlorobenzene is well established and modelled. The results indicate that total effective impact energy and reagent ratio are the two factors sufficient for describing the MC degradation degree of POPs. The reaction rate constant only depends on the chemical properties of reactants, so it could be used as an important index to appraise the quality of MC additives. This model successfully predicts the reaction rate for different operating conditions, indicating that it could be suitably applied for conducting MC reactions in other reactors.

Effect of selenium deficiency on the thermoelectric properties of n -type In 4 Se 3 - x compounds

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

Zhu, G. H.; Lan, Y. C.; Wang, H.

2011-03-01

Thermoelectric properties of dense bulk polycrystalline In 4 Se 3 - x ( x = 0, 0.25, 0.5, 0.65, and 0.8) compounds are investigated. A peak dimensionless thermoelectric figure of merit ( ZT ) of about 1 is achieved for x = 0.65 and 0.8. The peak ZT is about 50% higher than the previously reported highest value for polycrystalline In 4 Se 3 - x compounds. Our In 4 Se 3 - x samples were prepared by ball milling and hot pressing. We show that it is possible to effectively control the electrical conductivity and thermal conductivity by controllingmore » selenium (Se) deficiency x . The ZT enhancement is mainly attributed to the thermal conductivity reduction due to the increased phonon scattering by Se deficiency, defects, and nanoscale inclusions in the ball-milled and hot-pressed dense bulk In 4 Se 3 - x samples.« less

Effect of selenium deficiency on the thermoelectric properties of n-type In 4Se 3-x compounds

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

Zhu, G H; Lan, Y C; Wang, H

2011-03-04

Thermoelectric properties of dense bulk polycrystalline In 4Se 3-x (x = 0, 0.25, 0.5, 0.65, and 0.8) compounds are investigated. A peak dimensionless thermoelectric figure of merit (ZT) of about 1 is achieved for x = 0.65 and 0.8. The peak ZT is about 50% higher than the previously reported highest value for polycrystalline In 4Se 3-x} compounds. Our In 4Se 3-x samples were prepared by ball milling and hot pressing. We show that it is possible to effectively control the electrical conductivity and thermal conductivity by controlling selenium (Se) deficiency x. The ZT enhancement is mainly attributed to themore » thermal conductivity reduction due to the increased phonon scattering by Se deficiency, defects, and nanoscale inclusions in the ball-milled and hot-pressed dense bulk In 4Se 3-x samples.« less

The formation of ReS(2) inorganic fullerene-like structures containing Re(4) parallelogram units and metal-metal bonds.

PubMed

Coleman, Karl S; Sloan, Jeremy; Hanson, Neal A; Brown, Gareth; Clancy, Gerald P; Terrones, Mauricio; Terrones, Humberto; Green, Malcolm L H

2002-10-02

The encapsulation of ReO(x) within ReS(2) inorganic fullerene-like cages is described for the first time. The encapsulate was prepared by the sulfidization of both hand-milled and ball-milled samples of ReO(2); partial conversion of the oxide to the sulfide was achieved with the degree of sulfidization depending on the exposure to the sulfidizing agent, H(2)S.

Fabricating the spherical and flake silver powder used for the optoelectronic devices

NASA Astrophysics Data System (ADS)

Ju, Wei; Ma, Wangjing; Zhang, Fangzhi; Chen, Yixiang; Xie, Jinpeng

2018-01-01

The spherical and flake silver powder with different particle size for the optoelectronic devices was partly prepared by using chemical reduction and ball milling method, and charactered by scanning electron microscope (SEM), X-ray diffraction (XRD), laser particle size analyzer and thermo-gravimetric(TG) analyzer. The particle size of three series of spherical silver powder fabricated by chemical reduction is about 1.5μm, 1μm and 0.6μm, respectively; after being mechanical milling, the particle size of flake silver powder with high flaky rate is about 10μm, 6μm and 2μm respectively. Thermo gravimetric (TG) and XRD analyses showed that the silver powders have high purity and crystalline, and then the laser particle size and SEM analyses showed that the silver powders has good uniformity.

Structure and magnetic properties of low-temperature phase Mn-Bi nanosheets with ultra-high coercivity and significant anisotropy

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

Liu, Rongming, E-mail: rmliu@iphy.ac.cn, E-mail: shenbg@iphy.ac.cn; Zhang, Ming; Niu, E

2014-05-07

The microstructure, crystal structure, and magnetic properties of low-temperature phase (LTP) Mn-Bi nanosheets, prepared by surfactant assistant high-energy ball milling (SA-HEBM) with oleylamine and oleic acid as the surfactant, were examined with scanning electron microscopy, X-ray diffraction, and vibrating sample magnetometer, respectively. Effect of ball-milling time on the coercivity of LTP Mn-Bi nanosheets was systematically investigated. Results show that the high energy ball milling time from tens of minutes to several hours results in the coercivity increase of Mn-Bi powders and peak values of 14.3 kOe around 10 h. LTP Mn-Bi nanosheets are characterized by an average thickness of tensmore » of nanometers, an average diameter of ∼1.5 μm, and possess a relatively large aspect ratio, an ultra-high room temperature coercivity of 22.3 kOe, a significant geometrical and magnetic anisotropy, and a strong (00l) crystal texture. Magnetization and demagnetization behaviors reveal that wall pinning is the dominant coercivity mechanism in these LTP Mn-Bi nanosheets. The ultrafine grain refinement introduced by the SA-HEBM process contribute to the ultra-high coercivity of LTP Mn-Bi nanosheets and a large number of defects put a powerful pinning effect on the magnetic domain movement, simultaneously. Further magnetic measurement at 437 K shows that a high coercivity of 17.8 kOe and a strong positive temperature coefficient of coercivity existed in the bonded permanent magnet made by LTP Mn-Bi nanosheets.« less

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.

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.

Mechanochemical depolymerization of inulin.

PubMed

Xing, Haoran; Yaylayan, Varoujan A

2018-05-02

Although chemical reactions driven by mechanical force is emerging as a promising tool in the field of physical sciences, its applications in the area of food sciences are not reported. In this paper, we propose ball milling as an efficient tool for the controlled generation of fructooligosaccharide (FOS) mixtures from inulin with a degree of polymerization (dp) ranging between 4 and 7. The addition of catalytic amounts of AlCl 3 together with ball milling (30 min, at 30 Hz) generated mixtures rich in dehydrated disaccharides such as di-D-fructose dianhydrides. Based on anion exchange chromatography in conjunction with ESI/qTOF/MS/MS analysis, catalysis increased the overall content of mono-, di-, and tri-saccharides by around 30 fold compared to un-catalyzed milling. In addition, dialysis results of the untreated and treated samples have indicated that under catalysis the percent of depolymerization (dp < 12) reached 73.4% from the starting value of 27.6% in the untreated sample. Both processes resulted in mixtures of prebiotic value. The use of mechanical energy may be suitable for a fast, cost-efficient and green conversion of inulin to value-added food ingredients. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

Line profile analysis of ODS steels Fe20Cr5AlTiY milled powders at different Y2O3 concentrations

NASA Astrophysics Data System (ADS)

Afandi, A.; Nisa, R.; Thosin, K. A. Z.

2017-04-01

Mechanical properties of material are largely dictated by constituent microstructure parameters such as dislocation density, lattice microstrain, crystallite size and its distribution. To develop ultra-fine grain alloys such as Oxide Dispersion Strengthened (ODS) alloys, mechanical alloying is crucial step to introduce crystal defects, and refining the crystallite size. In this research the ODS sample powders were mechanically alloyed with different Y2O3 concentration respectively of 0.5, 1, 3, and 5 wt%. MA process was conducted with High Energy Milling (HEM) with the ball to powder ratio of 15:1. The vial and the ball were made of alumina, and the milling condition is set 200 r.p.m constant. The ODS powders were investigated by X-Ray Diffractions (XRD), Bragg-Brentano setup of SmartLab Rigaku with 40 KV, and 30 mA, step size using 0.02°, with scanning speed of 4°min-1. Line Profile Analysis (LPA) of classical Williamson-Hall was carried out, with the aim to investigate the different crystallite size, and microstrain due to the selection of the full wide at half maximum (FWHM) and integral breadth.

Modifications of Graphite and Multiwall Carbon Nanotubes in the Presence of Urea

NASA Astrophysics Data System (ADS)

Duraia, El-Shazly M.; Fahami, Abbas; Beall, Gary W.

2018-02-01

The effect of high-energy ball milling on two carbon allotropes, graphite and multiwall carbon nanotubes (MWCNT) in the presence of urea has been studied. Samples were investigated using Raman spectroscopy, x-ray diffraction, scanning electron microscope (SEM) and x-ray photoelectron spectroscopy (XPS). Nitrogen-doped graphene has been successfully synthesized via a simple scalable mechanochemistry method using urea and graphite powder precursors. XPS results revealed the existence of the different nitrogen atoms configurations including pyridine, pyrrodic and graphitic N. SEM observations showed that the graphene nanosheets morphology become more wrinkles folded and crumbled as the milling time increased. The ID/IG ratio also increased as the milling time rose. The presence of both D' and G + D bands at 1621 cm-1 and 2940 cm-1, respectively, demonstrated the nitrogen incorporation in the graphene lattice Two factors contribute to the used urea: first it helps to exfoliate graphite into graphene, and second it preserves the graphitic structure from damage during the milling process as well as acting as a solid-state nitrogen source. Based on the phase analysis, the d-spacing of MWCNT samples in the presence of urea decreased due to the mechanical force in the milling process as the milling time increased. On the other hand, in the graphite case, due to its open flat surface, the graphite (002) peak shifts toward lower two theta as the milling time increase. Such findings are important and could be used for large-scale production of N-doped graphene, diminishing the use of either dangerous chemicals or sophisticated equipment.

High yield fabrication of fluorescent nanodiamonds

PubMed Central

Boudou, Jean-Paul; Curmi, Patrick; Jelezko, Fedor; Wrachtrup, Joerg; Aubert, Pascal; Sennour, Mohamed; Balasubramanian, Gopalakrischnan; Reuter, Rolf; Thorel, Alain; Gaffet, Eric

2009-01-01

A new fabrication method to produce homogeneously fluorescent nanodiamonds with high yields is described. The powder obtained by high energy ball milling of fluorescent high pressure, high temperature diamond microcrystals was converted in a pure concentrated aqueous colloidal dispersion of highly crystalline ultrasmall nanoparticles with a mean size less than or equal to 10 nm. The whole fabrication yield of colloidal quasi-spherical nanodiamonds was several orders of magnitude higher than those previously reported starting from microdiamonds. The results open up avenues for the industrial cost-effective production of fluorescent nanodiamonds with well-controlled properties. PMID:19451687

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

Compact Process for the Preparation of Microfine Spherical High-Niobium-Containing TiAl Alloy Powders

NASA Astrophysics Data System (ADS)

Tong, J. B.; Lu, X.; Liu, C. C.; Wang, L. N.; Qu, X. H.

2015-03-01

High-Nb-containing TiAl alloys are a new generation of materials for high-temperature structural applications because of their superior high-temperature mechanical properties. The alloy powders can be widely used for additive manufacturing, thermal spraying, and powder metallurgy. Because of the difficulty of making microfine spherical alloy powders in quantity by conventional techniques, a compact method was proposed, which consisted of two-step ball milling of elemental powders and subsequent radio frequency (RF) argon plasma spheroidization. In comparison with conventional mechanical alloying techniques, the two-step milling process can be used to prepare alloy powders with uniform scale in a short milling time with no addition of process control agent. This makes the process effective and less contaminating. After RF argon plasma spheroidization, the powders produced exhibit good sphericity, and the number-average diameter is about 8.2 μm with a symmetric unimodal particle size distribution. The powders perform high composition homogeneity and contain predominately supersaturated α 2-Ti3Al phase. The oxygen and carbon contents of the spheroidized powder are 0.47% and 0.050%, respectively.

Hydrogen Decrepitation Press-Less Process recycling of NdFeB sintered magnets

NASA Astrophysics Data System (ADS)

Xia, Manlong; Abrahamsen, Asger B.; Bahl, Christian R. H.; Veluri, Badrinath; Søegaard, Allan I.; Bøjsøe, Poul

2017-11-01

A Hydrogen Decrepitation Press-Less Process (HD-PLP) recycling method for recycling of anisotropic NdFeB magnets is demonstrated. The method combines hydrogen decrepitation (HD) disintegration of the initial magnet, powder sieving and the Press-Less Process (PLP), where hydride powder is sintered in a graphite mold. Coercivities up to 534 kA/m were obtained in porous samples based on powder size d < 100 μm. Adding a ball milling step resulted in full density isotropic magnets for d > 100 μm. The coercivity reached Hci = 957 kA/m being 86% of the original N48M material without addition of rare earth elements.

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.

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.

Short communication: investigating the effect of saffron (Crocus sativus L.) nano-sizing on its colour extraction efficiency: a preliminary study.

PubMed

Abootalebian, Mehrdad; Karbasi, Maryam; Sadeghi, Maliheh; Abdinian, Mahnaz; Polikarpov, Igor

2017-10-01

This study investigated the effect of saffron nano-sizing on its the colour extraction yield. The whole stigma was ball-milled at three different times (10, 20 and 100 h), immediately or with a 24 h delay was submitted to absorption test, and then the colour extraction efficiency was determined. When stigma was milled for 100 h, its particle size was reduced to less than 20 nm, as shown by SEM and TEM images, and its extraction efficiency was considerably increased by 19.8% as compared with the stigma blended for 10 min. However with a 24 h delay between the end of milling and absorption test, the yield of colour extraction significantly decreased. The recommended milling conditions resulting in extraction efficiency of 16.2% (in comparison with stigma blended for 10 min) were determined to be the milling for 10 h with initial tendering prior to milling operation.

Fabrication of an r-Al2Ti intermetallic matrix composite reinforced with α-Al2O3 ceramic by discontinuous mechanical milling for thermite reaction

NASA Astrophysics Data System (ADS)

Mosleh, A.; Ehteshamzadeh, M.; Taherzadeh Mousavian, R.

2014-10-01

In this study, a powder mixture with an Al/TiO2 molar ratio of 10/3 was used to form an r-Al2Ti intermetallic matrix composite (IMC) reinforced with α-Al2O3 ceramic by a novel milling technique, called discontinuous mechanical milling (DMM) instead of milling and ignition of the produced thermite. The results of energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) of samples with varying milling time indicate that this fabrication process requires considerable mechanical energy. It is shown that Al2Ti-Al2O3 IMC with small grain size was produced by DMM after 15 h of ball milling. Peaks for γ-TiAl as well as Al2Ti and Al2O3 are observed in XRD patterns after DMM followed by heat treatment. The microhardness of the DMM-treated composite produced after heat treatment was higher than Hv 700.

Hydrogen storage materials and method of making by dry homogenation

DOEpatents

Jensen, Craig M.; Zidan, Ragaiy A.

2002-01-01

Dry homogenized metal hydrides, in particular aluminum hydride compounds, as a material for reversible hydrogen storage is provided. The reversible hydrogen storage material comprises a dry homogenized material having transition metal catalytic sites on a metal aluminum hydride compound, or mixtures of metal aluminum hydride compounds. A method of making such reversible hydrogen storage materials by dry doping is also provided and comprises the steps of dry homogenizing metal hydrides by mechanical mixing, such as be crushing or ball milling a powder, of a metal aluminum hydride with a transition metal catalyst. In another aspect of the invention, a method of powering a vehicle apparatus with the reversible hydrogen storage material is provided.

Highly reliable field electron emitters produced from reproducible damage-free carbon nanotube composite pastes with optimal inorganic fillers.

PubMed

Kim, Jae-Woo; Jeong, Jin-Woo; Kang, Jun-Tae; Choi, Sungyoul; Ahn, Seungjoon; Song, Yoon-Ho

2014-02-14

Highly reliable field electron emitters were developed using a formulation for reproducible damage-free carbon nanotube (CNT) composite pastes with optimal inorganic fillers and a ball-milling method. We carefully controlled the ball-milling sequence and time to avoid any damage to the CNTs, which incorporated fillers that were fully dispersed as paste constituents. The field electron emitters fabricated by printing the CNT pastes were found to exhibit almost perfect adhesion of the CNT emitters to the cathode, along with good uniformity and reproducibility. A high field enhancement factor of around 10,000 was achieved from the CNT field emitters developed. By selecting nano-sized metal alloys and oxides and using the same formulation sequence, we also developed reliable field emitters that could survive high-temperature post processing. These field emitters had high durability to post vacuum annealing at 950 °C, guaranteeing survival of the brazing process used in the sealing of field emission x-ray tubes. We evaluated the field emitters in a triode configuration in the harsh environment of a tiny vacuum-sealed vessel and observed very reliable operation for 30 h at a high current density of 350 mA cm(-2). The CNT pastes and related field emitters that were developed could be usefully applied in reliable field emission devices.

Highly reliable field electron emitters produced from reproducible damage-free carbon nanotube composite pastes with optimal inorganic fillers

NASA Astrophysics Data System (ADS)

Kim, Jae-Woo; Jeong, Jin-Woo; Kang, Jun-Tae; Choi, Sungyoul; Ahn, Seungjoon; Song, Yoon-Ho

2014-02-01

Highly reliable field electron emitters were developed using a formulation for reproducible damage-free carbon nanotube (CNT) composite pastes with optimal inorganic fillers and a ball-milling method. We carefully controlled the ball-milling sequence and time to avoid any damage to the CNTs, which incorporated fillers that were fully dispersed as paste constituents. The field electron emitters fabricated by printing the CNT pastes were found to exhibit almost perfect adhesion of the CNT emitters to the cathode, along with good uniformity and reproducibility. A high field enhancement factor of around 10 000 was achieved from the CNT field emitters developed. By selecting nano-sized metal alloys and oxides and using the same formulation sequence, we also developed reliable field emitters that could survive high-temperature post processing. These field emitters had high durability to post vacuum annealing at 950 °C, guaranteeing survival of the brazing process used in the sealing of field emission x-ray tubes. We evaluated the field emitters in a triode configuration in the harsh environment of a tiny vacuum-sealed vessel and observed very reliable operation for 30 h at a high current density of 350 mA cm-2. The CNT pastes and related field emitters that were developed could be usefully applied in reliable field emission devices.

Processing of AlCoCrFeNiTi high entropy alloy by atmospheric plasma spraying

NASA Astrophysics Data System (ADS)

Löbel, M.; Lindner, T.; Kohrt, C.; Lampke, T.

2017-03-01

High Entropy Alloys (HEA) are gaining increasing interest due to their unique combination of properties. Especially the combination of high mechanical strength and hardness with distinct ductility makes them attractive for numerous applications. One interesting alloy system that exhibits excellent properties in bulk state is AlCoCrFeNiTi. A high strength, wear resistance and high-temperature resistance are the necessary requirements for the application in surface engineering. The suitability of blended, mechanically ball milled and inert gas atomized feedstock powders for the development of atmospheric plasma sprayed (APS) coatings is investigated in this study. The ball milled and inert gas atomized powders were characterized regarding their particle morphology, phase composition, chemical composition and powder size distribution. The microstructure and phase composition of the thermal spray coatings produced with different feedstock materials was investigated and compared with the feedstock material. Furthermore, the Vickers hardness (HV) was measured and the wear behavior under different tribological conditions was tested in ball-on-disk, oscillating wear and scratch tests. The results show that all produced feedstock materials and coatings exhibit a multiphase composition. The coatings produced with inert gas atomized feedstock material provide the best wear resistance and the highest degree of homogeneity.

Confined NaAlH4 nanoparticles inside CeO2 hollow nanotubes towards enhanced hydrogen storage.

PubMed

Gao, Qili; Xia, Guanglin; Yu, Xuebin

2017-10-05

NaAlH 4 has been widely regarded as a potential hydrogen storage material due to its favorable thermodynamics and high energy density. The high activation energy barrier and high dehydrogenation temperature, however, significantly hinder its practical application. In this paper, CeO 2 hollow nanotubes (HNTs) prepared by a simple electrospinning technique are adopted as functional scaffolds to support NaAlH 4 nanoparticles (NPs) towards advanced hydrogen storage performance. The nanoconfined NaAlH 4 inside CeO 2 HNTs, synthesized via the infiltration of molten NaAlH 4 into the CeO 2 HNTs under high hydrogen pressure, exhibited significantly improved dehydrogenation properties compared with both bulk and ball-milled CeO 2 HNTs-catalyzed NaAlH 4 . The onset dehydrogenation temperature of the NaAlH 4 @CeO 2 composite was reduced to below 100 °C, with only one main dehydrogenation peak appearing at 130 °C, which is 120 °C and 50 °C lower than for its bulk counterpart and for the ball-milled CeO 2 HNTs-catalyzed NaAlH 4 , respectively. Moreover, ∼5.09 wt% hydrogen could be released within 30 min at 180 °C, while only 1.6 wt% hydrogen was desorbed from the ball-milled NaAlH 4 under the same conditions. This significant improvement is mainly attributed to the synergistic effects contributed by the CeO 2 HNTs, which could act as not only a structural scaffold to fabricate and confine the NaAlH 4 NPs, but also as an effective catalyst to enhance the hydrogen storage performance of NaAlH 4 .

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.

Mechanochemistry of nucleosides, nucleotides and related materials

PubMed Central

Eguaogie, Olga; Conlon, Patrick F; Gîlea, Manuela A; Liang, Yipei

2018-01-01

The application of mechanical force to induce the formation and cleavage of covalent bonds is a rapidly developing field within organic chemistry which has particular value in reducing or eliminating solvent usage, enhancing reaction rates and also in enabling the preparation of products which are otherwise inaccessible under solution-phase conditions. Mechanochemistry has also found recent attention in materials chemistry and API formulation during which rearrangement of non-covalent interactions give rise to functional products. However, this has been known to nucleic acids science almost since its inception in the late nineteenth century when Miescher exploited grinding to facilitate disaggregation of DNA from tightly bound proteins through selective denaturation of the latter. Despite the wide application of ball milling to amino acid chemistry, there have been limited reports of mechanochemical transformations involving nucleoside or nucleotide substrates on preparative scales. A survey of these reactions is provided, the majority of which have used a mixer ball mill and display an almost universal requirement for liquid to be present within the grinding vessel. Mechanochemistry of charged nucleotide substrates, in particular, provides considerable benefits both in terms of efficiency (reducing total processing times from weeks to hours) and by minimising exposure to aqueous conditions, access to previously elusive materials. In the absence of large quantities of solvent and heating, side-reactions can be reduced or eliminated. The central contribution of mechanochemistry (and specifically, ball milling) to the isolation of biologically active materials derived from nuclei by grinding will also be outlined. Finally non-covalent associative processes involving nucleic acids and related materials using mechanochemistry will be described: specifically, solid solutions, cocrystals, polymorph transitions, carbon nanotube dissolution and inclusion complex formation. PMID:29765475

Fast sodium ionic conduction in Na2B10H10-Na2B12H12 pseudo-binary complex hydride and application to a bulk-type all-solid-state battery

NASA Astrophysics Data System (ADS)

Yoshida, Koji; Sato, Toyoto; Unemoto, Atsushi; Matsuo, Motoaki; Ikeshoji, Tamio; Udovic, Terrence J.; Orimo, Shin-ichi

2017-03-01

In the present work, we developed highly sodium-ion conductive Na2B10H10-Na2B12H12 pseudo-binary complex hydride via mechanically ball-milling admixtures of the pure Na2B10H10 and Na2B12H12 components. Both of these components show a monoclinic phase at room temperature, but ball-milled mixtures partially stabilized highly ion-conductive, disordered cubic phases, whose fraction and favored structural symmetry (body-centered cubic or face-centered cubic) depended on the conditions of mechanical ball-milling and molar ratio of the component compounds. First-principles molecular-dynamics simulations demonstrated that the total energy of the closo-borane mixtures and pure materials is quite close, helping to explain the observed stabilization of the mixed compounds. The ionic conductivity of the closo-borane mixtures appeared to be correlated with the fraction of the body-centered-cubic phase, exhibiting a maximum at a molar ratio of Na2B10H10:Na2B12H12 = 1:3. A conductivity as high as log(σ/S cm-1) = -3.5 was observed for the above ratio at 303 K, being approximately 2-3 orders of magnitude higher than that of either pure material. A bulk-type all-solid-state sodium-ion battery with a closo-borane-mixture electrolyte, sodium-metal negative-electrode, and TiS2 positive-electrode demonstrated a high specific capacity, close to the theoretical value of NaTiS2 formation and a stable discharge/charge cycling for at least eleven cycles, with a high discharge capacity retention ratio above 91% from the second cycle.

Synthesis and Characterization of Iron Doped Nano Barium Titanate Through Mechanochemical Route

NASA Astrophysics Data System (ADS)

Mukherjee, Soumya; Ghosh, S.; Ghosh, C.; Mitra, M. K.

2013-04-01

Mechanochemical activation was used to prepare Fe doped barium titanate with intense milling in high energy planetary ball mill. Calcination was done at 1250°C for 30 min to obtain BaO, followed by milling with titania, at 400 rpm for 3 and 6 h. Ferric oxide was used for Fe doping. Annealing was done on the milled sample at 650, 750 and 850 °C for 3 and 6 h to generate stoichiometric compound of barium titanate phase. Fe doped barium titanate results in dense cluster of irregular polygonal shape morphology while morphology was spherical in nature for undoped sample. UV-VIS spectra analysis was carried out to determine bandgap (3.93 eV for undoped BT and 3.88 eV for Fe doped BT) followed by emission-excitation of the sample by fluorometric analysis.

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.

Hydrogen storage properties of Mg xFe (x: 2, 3 and 15) compounds produced by reactive ball milling

NASA Astrophysics Data System (ADS)

Puszkiel, J. A.; Arneodo Larochette, P.; Gennari, F. C.

This work deals with the assessment of the thermo-kinetic properties of Mg-Fe based materials for hydrogen storage. Samples are prepared from Mg xFe (x: 2, 3 and 15) elemental powder mixtures via low energy ball milling under hydrogen atmosphere at room temperature. The highest yield is obtained with Mg 15Fe after 150 h of milling (90 wt% of MgH 2). The thermodynamic characterization carried out between 523 and 673 K shows that the obtained Mg-Fe-H hydride systems have similar thermodynamic parameters, i.e. enthalpy and entropy. However, in equilibrium conditions, Mg 15Fe has higher hydrogen capacity and small hysteresis. In dynamic conditions, Mg 15Fe also shows better hydrogen capacity (4.85 wt% at 623 K absorbed in less than 10 min and after 100 absorption/desorption cycles), reasonably good absorption/desorption times and cycling stability in comparison to the other studied compositions. From hydrogen uptake rate measurements performed at 573 and 623 K, the rate-limiting step of the hydrogen uptake reaction is determined by fitting particle kinetic models. According to our results, the hydrogen uptake is diffusion controlled, and this mechanism does not change with the Mg-Fe proportion and temperature.

Enhanced thermoelectric performance realized in AgBiS2 composited AgBiSe2 through indium doping and mechanical alloying

NASA Astrophysics Data System (ADS)

Guan, Yingdong; Huang, Yi; Wu, Di; Feng, Dan; He, Mingkai; He, Jiaqing

2018-05-01

AgBiSe2 is deemed as a decent candidate of state-of-arts thermoelectric lead chalcogenides due to its intrinsically low lattice thermal conductivity. In this work, we report that a peak figure of merit of ˜0.9 can be realized at 773 K in n-type AgBiSe2 when it is simultaneously doped with indium and composited with AgBiS2 through the ball milling process. The enhancement of thermoelectric performance of AgBiSe2 largely comes from the significant reduction of thermal conductivity from ˜0.5 W/mK to 0.33 W/mK at 773 K, which is the record low value ever reported in this specific system. The decrease in thermal conductivity can be ascribed to the combination of grain size reduction and enhanced alloy scattering from S-Se substitution during the high energy ball milling processes.

Particle size dependence on magnetic and electrical properties of (Ni0.8Fe0.2)10C90 granular composites.

PubMed

Mandal, Guruprasad; Srinivas, V; Rao, V V

2011-03-01

The granular structure and electrical transport behavior of ball milled magnetic permalloy particles and graphite forming (Ni0.8Fe0.2)10C90 granular composites have been reported. Retaining the composite composition to be 90:10 and varying the particle size of permalloy, the electronic transport properties have been carried out down to 4 K under the external applied magnetic field of 50 kOe. All the samples show semiconducting like behavior and positive magnetoresistance (MR) in the temperature range 4-300 K. A strong anisotropic magnetoresistance in these samples has also been observed. The highest 31% longitudinal and 6.8% transverse magnetoresistance values have been observed in 40 hrs ball milled (Ni0.8Fe0.2)10C90 composite. From these studies, we suggest that the magnetic component present in the sample may not be playing a major role in obtaining large positive MR values, which is in deviation with the earlier reports.

Preparation of powders suitable for conversion to useful .beta.-aluminas

DOEpatents

Morgan, Peter E. D.

1982-01-01

A process for forming a precursor powder which, when suitably pressed and sintered forms highly pure, densified .beta.- or .beta."-alumina, comprising the steps of: (1) forming a suspension (or slurry) of Bayer-derived Al(OH).sub.3 in a water-miscible solvent; (2) adding an aqueous solution of a Mg compound, a Li compound, a Na compound or mixtures thereof to the Bayer-derived Al(OH).sub.3 suspension while agitating the mixture formed thereby, to produce a gel; (3) drying the gel at a temperature above the normal boiling point of water to produce a powder material; (4) lightly ball milling and sieving said powder material; and (5) heating the ball-milled and sieved powder material at a temperature of between 350.degree. to 900.degree. C. to form the .beta.- or .beta."-alumina precursor powder. The precursor powder, thus formed, may be subsequently isopressed at a high pressure and sintered at an elevated temperature to produce .beta.- or .beta."-alumina. BACKGROUND OF THE INVENTION

Effects of intergranular phase on the coercivity for MnBi magnets prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Cao, J.; Huang, Y. L.; Hou, Y. H.; Zhang, G. Q.; Shi, Z. Q.; Zhong, Z. C.; Liu, Z. W.

2018-05-01

MnBi magnets with a high content of low temperature phase (LTP) and excellent magnetic properties were prepared by spark plasma sintering (SPS) using ball milling powders as precursors without magnetic purification. A complicated intergranular phase, which contains Mn phase, Bi phase, MnO phase, and even amorphous phase in MnBi magnets, was characterized and reported systematically. It was found that the formation of intergranular phase which was contributed by ball milling precursors and sintering mechanism, jointly, had important influence on the magnetic properties. The appropriate content of intergranular phase was beneficial in improving the coercivity due to the strong magnetic isolation effects. The optimum magnetic properties with Mr=26.0 emu/g, Hci= 7.11 kOe and (BH)max=1.53 MGOe at room temperature, and a maximum value Hci= 25.37 kOe at 550 K can be obtained. Strongly favorable magnetic properties make SPSed MnBi magnets an attractive candidate material for small permanent magnets used in high-temperature applications.

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.

Two-dimensional distribution of carbon nanotubes in copper flake powders.

PubMed

Tan, Zhanqiu; Li, Zhiqiang; Fan, Genlian; Li, Wenhuan; Liu, Qinglei; Zhang, Wang; Zhang, Di

2011-06-03

We report an approach of flake powder metallurgy to the uniform, two-dimensional (2D) distribution of carbon nanotubes (CNTs) in Cu flake powders. It consists of the preparation of Cu flakes by ball milling in an imidazoline derivative (IMD) aqueous solution, surface modification of Cu flakes with polyvinyl alcohol (PVA) hydrosol and adsorption of CNTs from a CNT aqueous suspension. During ball milling, a hydrophobic monolayer of IMD is adsorbed on the surface of the Cu flakes, on top of which a hydrophilic PVA film is adsorbed subsequently. This PVA film could further interact with the carboxyl-group functionalized CNTs and act to lock the CNTs onto the surfaces of the Cu flakes. The CNT volume fraction is controlled easily by adjusting the concentration/volume of CNT aqueous suspension and Cu flake thickness. The as-prepared CNT/Cu composite flakes will serve as suitable building blocks for the self-assembly of CNT/Cu laminated composites that enable the full potential of 2D distributed CNTs to achieve high thermal conductivity.

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.

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.

Gas Release Behavior of Cu-TiH2 Composite Powder and Its Application as a Blowing Agent to Fabricate Aluminum Foams with Low Porosity and Small Pore Size

NASA Astrophysics Data System (ADS)

Cheng, Ying; Li, Yanxiang; Chen, Xiang; Liu, Zhiyong; Zhou, Xu; Wang, Ningzhen

2018-06-01

Compared to traditional pore structure with high porosity (≥ 80 pct) and large pore size (≥ 3 mm), aluminum foams with low porosity (60 to 70 pct) and small pore size (≤ 2 mm) possess higher compressive property and formability. In order to achieve the goal of reducing pore size, Cu-TiH2 composite powder prepared by ball milling preoxidized TiH2 with Cu powder was used as a blowing agent. Its gas release behavior was characterized by thermogravimetric analysis and differential scanning calorimetry. The results show that the ball milling treatment can advance the gas release process and slow the gas release rate at the same time. All these changes are favorable to the reduction of porosity and pore size. Such Cu-TiH2 composite powder provides an alternative way to fabricate aluminum foams with low porosity and small pore size.

A new technique for the strengthening of aluminum tungsten inert gas weld metals: using carbon nanotube/aluminum composite as a filler metal.

PubMed

Fattahi, M; Nabhani, N; Rashidkhani, E; Fattahi, Y; Akhavan, S; Arabian, N

2013-01-01

The effect of multi-walled carbon nanotube (MWCNT) on the mechanical properties of aluminum multipass weld metal prepared by the tungsten inert gas (TIG) welding process was investigated. High energy ball milling was used to disperse MWCNT in the aluminum powder. Carbon nanotube/aluminum composite filler metal was fabricated for the first time by hot extrusion of ball-milled powders. After welding, the tensile strength, microhardness and MWCNT distribution in the weld metal were investigated. The test results showed that the tensile strength and microhardness of weld metal was greatly increased when using the filler metal containing 1.5 wt.% MWCNT. Therefore, according to the results presented in this paper, it can be concluded that the filler metal containing MWCNT can serve as a super filler metal to improve the mechanical properties of TIG welds of Al and its alloys. Copyright © 2013 Elsevier Ltd. All rights reserved.

Impact Load Behavior between Different Charge and Lifter in a Laboratory-Scale Mill

PubMed Central

Yin, Zixin; Zhu, Zhencai; Yu, Zhangfa; Li, Tongqing

2017-01-01

The impact behavior between the charge and lifter has significant effect to address the mill processing, and is affected by various factors including mill speed, mill filling, lifter height and media shape. To investigate the multi-body impact load behavior, a series of experiments and Discrete Element Method (DEM) simulations were performed on a laboratory-scale mill, in order to improve the grinding efficiency and prolong the life of the lifter. DEM simulation hitherto has been extensively applied as a leading tool to describe diverse issues in granular processes. The research results shown as follows: The semi-empirical power draw of Bond model in this paper does not apply very satisfactorily for the ball mills, while the power draw determined by DEM simulation show a good approximation for the measured power draw. Besides, the impact force on the lifter was affected by mill speed, grinding media filling, lifter height and iron ore particle. The maximum percent of the impact force between 600 and 1400 N is at 70–80% of critical speed. The impact force can be only above 1400 N at the grinding media filling of 20%, and the maximum percent of impact force between 200 and 1400 N is obtained at the grinding media filling of 20%. The percent of impact force ranging from 0 to 200 N decreases with the increase of lifter height. However, this perfect will increase above 200 N. The impact force will decrease when the iron ore particles are added. Additionally, for the 80% of critical speed, the measured power draw has a maximum value. Increasing the grinding media filling increases the power draw and increasing the lifter height does not lead to any variation in power draw. PMID:28773243

Impact Load Behavior between Different Charge and Lifter in a Laboratory-Scale Mill.

PubMed

Yin, Zixin; Peng, Yuxing; Zhu, Zhencai; Yu, Zhangfa; Li, Tongqing

2017-07-31

The impact behavior between the charge and lifter has significant effect to address the mill processing, and is affected by various factors including mill speed, mill filling, lifter height and media shape. To investigate the multi-body impact load behavior, a series of experiments and Discrete Element Method (DEM) simulations were performed on a laboratory-scale mill, in order to improve the grinding efficiency and prolong the life of the lifter. DEM simulation hitherto has been extensively applied as a leading tool to describe diverse issues in granular processes. The research results shown as follows: The semi-empirical power draw of Bond model in this paper does not apply very satisfactorily for the ball mills, while the power draw determined by DEM simulation show a good approximation for the measured power draw. Besides, the impact force on the lifter was affected by mill speed, grinding media filling, lifter height and iron ore particle. The maximum percent of the impact force between 600 and 1400 N is at 70-80% of critical speed. The impact force can be only above 1400 N at the grinding media filling of 20%, and the maximum percent of impact force between 200 and 1400 N is obtained at the grinding media filling of 20%. The percent of impact force ranging from 0 to 200 N decreases with the increase of lifter height. However, this perfect will increase above 200 N. The impact force will decrease when the iron ore particles are added. Additionally, for the 80% of critical speed, the measured power draw has a maximum value. Increasing the grinding media filling increases the power draw and increasing the lifter height does not lead to any variation in power draw.

On the formation and stability of nanometer scale precipitates in ferritic alloys during processing and high temperature service

NASA Astrophysics Data System (ADS)

Alinger, Matthew J.

Iron powders containing ≈14wt%Cr and smaller amounts of W and Ti were mechanically alloyed (MA) by ball milling with Y2O3 and subsequently either hot consolidated by hot extrusion or isostatic pressing, or powder annealed, producing very high densities of nm-scale coherent transition phase precipitates, or Y-Ti-O nano-clusters (NCs), along with fine-scale grains. These so-called nanostructured ferritic alloys (NFAs) manifest very high strength (static and creep) and corrosion-oxidation resistance up to temperatures in excess of 800°C. We used a carefully designed matrix of model MA powders and consolidated alloys to systematically assess the NC evolutions during each processing step, and to explore the combined effects of alloy composition and a number of processing variables, including the milling energy, consolidation method and the time and temperature of annealing of the as-milled powders. The stability of the NCs was also characterized during high-temperate post-consolidation annealing of a commercial NFA, MA957. The micro-nanostructural evolutions, and their effects on the alloy strength, were characterized by a combination of techniques, including XRD, TEM, atom-probe tomography (APT) and positron annihilation spectroscopy (PAS). However, small angle neutron scattering (SANS) was the primary tool used to characterize the nm-scale precipitates. The effect of the micro-nanostructure on the alloy strength was assessed by microhardness measurements. The studies revealed the critical sequence-of-events in forming the NCs, involves dissolution of Y, Ti and O during ball milling. The supersaturated solutes then precipitate during hot consolidation or powder annealing. The precipitate volume fraction increases with both the milling energy and Ti additions at lower consolidation and annealing temperatures (850°C), and at higher processing temperatures (1150°C) both are needed to produce NCs. The non-equilibrium kinetics of NC formation are nucleation controlled and independent of time with an effective activation energy of ≈60 kJ/mole. High temperature precipitate coarsening and transformations to oxide phases show a high effective activation energy (≈880 kJ/mole) and have a time dependence characteristic of a dislocation pipe diffusion mechanism. The NCs act as weak to moderately strong (alpha = 0.1 to 0.5) obstacles that can be sheared by dislocations, where the obstacle strength increases with alpha ≈0.37log(r/2b).

Porosity Dependence of Piezoelectric Properties for Porous Potassium Niobate System Ceramics

NASA Astrophysics Data System (ADS)

Wada, S.; Mase, Y.; Shimizu, S.; Maeda, K.; Fujii, I.; Nakashima, K.; Pulpan, P.; Miyajima, N.

2011-10-01

Porous potassium niobate (KNbO3, KN) system ceramics were prepared by a conventional sintering method using carbon black (CB) nanoparticles. First, KN nanoparticles with a size of 100 nm was mixed with CB nanoparticles and binder using ball milling with ethanol. The mixture was dried, and pressed into pellets using uniaxial pressing. After binder burnout, these ceramics was sintered in air. Their piezoelectric properties were measured and discussed a relationship between porosity and piezoelectric properties. As the results, with increasing porosity, piezoelectric g33 constant increased significantly, which suggested that porous ceramics were effective for stress sensor application.

Low-temperature rapid synthesis and superconductivity of Fe-based oxypnictide superconductors.

PubMed

Fang, Ai-Hua; Huang, Fu-Qiang; Xie, Xiao-Ming; Jiang, Mian-Heng

2010-03-17

Fe-based oxypnictide superconductors were successfully synthesized at lower reaction temperatures and with shorter reaction times made possible by starting with less stable compounds, which provide a larger driving force for reactions. Using ball-milled powders of intermediate compounds, phase-pure superconductors with T(c) above 50 K were synthesized at 1173 K in 20 min. This method is particularly advantageous for retaining F, a volatile dopant that enhances superconductivity. Bulk superconductivity and high upper critical fields up to 392 T in Sm(0.85)Nd(0.15)FeAsO(0.85)F(0.15) were demonstrated.

An easy access to nanocrystalline alkaline earth metal fluorides - just by shaking

NASA Astrophysics Data System (ADS)

Dreger, M.; Scholz, G.; Kemnitz, E.

2012-04-01

High energy ball milling as fast, direct and solvent free method allows an easy access to nanocrystalline alkaline earth metal fluorides MF2 (M: Mg, Ca, Sr, Ba). Comparable metal sources (acetates, carbonates, hydroxides, alkoxides) were used for the reaction with NH4F as fluorinating agent. Even very simple manual shaking experiments between NH4F and the corresponding hydroxides in the stoichiometric ratio (M:F = 1:2, M: Ca, Sr, Ba) give phase pure fluorides. Moreover, comparable classical thermal reactions in closed crucibles at higher temperatures provide phase pure crystalline fluorides in nearly all cases as well.

Iron-based amorphous alloys and methods of synthesizing iron-based amorphous alloys

DOEpatents

Saw, Cheng Kiong; Bauer, William A.; Choi, Jor-Shan; Day, Dan; Farmer, Joseph C.

2016-05-03

A method according to one embodiment includes combining an amorphous iron-based alloy and at least one metal selected from a group consisting of molybdenum, chromium, tungsten, boron, gadolinium, nickel phosphorous, yttrium, and alloys thereof to form a mixture, wherein the at least one metal is present in the mixture from about 5 atomic percent (at %) to about 55 at %; and ball milling the mixture at least until an amorphous alloy of the iron-based alloy and the at least one metal is formed. Several amorphous iron-based metal alloys are also presented, including corrosion-resistant amorphous iron-based metal alloys and radiation-shielding amorphous iron-based metal alloys.

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.

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.

Optimization of the Technological Synthesis of Refractory Compounds

NASA Astrophysics Data System (ADS)

Gaidar, S. M.; Karelina, M. Yu.; Prikhod'ko, V. M.; Volkov, A. A.

2017-12-01

The results of experimental studies, which are related to the regulation of the fractional composition of refractory compounds by roll milling in using controlled roll opening and unbalanced peripheral speeds of rollers, are reported. The content of prepared fine, middle, and coarse fractions is within 50-80%; in this case, the milling time of synthesis products is less than the time of ball milling by an order of magnitude. The application of roll milling for refining the products of self-propagating high-temperature synthesis can be most efficient in using together with heat-generating reactor to solve the main problem of self-propagating synthesis (SHS), which is a problem for recent several decades (the problem is the creation of intense automated production of refractory compounds in using continuous manufacturing cycle within a energotechnological system with the recovery of a great quantity of heat released during SHS).

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

Exfoliation of graphene sheets via high energy wet milling of graphite in 2-ethylhexanol and kerosene.

PubMed

Al-Sherbini, Al-Sayed; Bakr, Mona; Ghoneim, Iman; Saad, Mohamed

2017-05-01

Graphene sheets have been exfoliated from bulk graphite using high energy wet milling in two different solvents that were 2-ethylhexanol and kerosene. The milling process was performed for 60 h using a planetary ball mill. Morphological characteristics were investigated using scanning electron microscope (SEM) and transmission electron microscope (TEM). On the other hand, the structural characterization was performed using X-ray diffraction technique (XRD) and Raman spectrometry. The exfoliated graphene sheets have represented good morphological and structural characteristics with a valuable amount of defects and a good graphitic structure. The graphene sheets exfoliated in the presence of 2-ethylhexanol have represented many layers, large crystal size and low level of defects, while the graphene sheets exfoliated in the presence of kerosene have represented fewer number of layers, smaller crystal size and higher level of defects.

Synthesis and characterization of nanocrystalline Al 2024-B4C composite powders by mechanical alloying

NASA Astrophysics Data System (ADS)

Varol, T.; Canakci, A.

2013-06-01

In the present work, the effect of milling parameters on the morphology and microstructure of nanostructure Al2024-B4C composite powders obtained by mechanical alloying (MA) was studied. The effects of milling time and B4C content on the morphology, microstructure and particle size of nanostructure Al2024-B4C composite powders have been investigated. Different amounts of B4C particles (0, 5, 10 and 20 wt.%) were mixed with Al2024 powders and milled in a planetary ball mill for 30, 60, 120, 300, 420 and 600 min. Al 2024-B4C composite powders were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, X-ray diffraction analysis (XRD) and the Vickers microhardness test. The results showed that the nanostructure Al2024-B4C composite powders were produced when they were milled for 600 min. The size of composite powder in the milled powder mixture was affected by the milling time and content of B4C particles. Moreover, it was observed that when MA reached a steady state, the properties of composite powders were stabilized.

Optimizing particle size reduction of biochar using a planetary ball mill

USDA-ARS?s Scientific Manuscript database

With world demand for fossil fuels consistently growing, reducing our dependence on petroleum products is a necessary strategy. Our research group is currently studying the feasibility of biochar as rubber composite filler. If biochar can be used as a partial or complete substitute for carbon black ...

Increasing biochar surface area: Optimization of ball milling parameters

USDA-ARS?s Scientific Manuscript database

Biochar produced from corn stover is a renewable, plentiful source of carbon that is a potential substitute for carbon black as rubber composite filler and also as binder/filter media for water or beverage purification applications. However, to be successful in these applications, the surface area o...

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

Rather, Sami ullah, E-mail: rathersami@gmail.com; Taimoor, Aqeel Ahmad; Muhammad, Ayyaz

Highlights: • Hydrogen adsorption comparisons of commercial, milled, and MgH{sub 2} composite. • Hydrogen adsorption capacity and kinetics improves tremendously by CNT embedding. • Unsteady state modeling and simulation of adsorption kinetics. - Abstract: Magnesium hydride (MgH{sub 2})–carbon nanotubes (CNT) composite has been prepared by high-energy ball milling method and their experimental and kinetic hydrogen adsorption studies was assessed. Hydrogen adsorption studies were performed by Sievert’s volumetric apparatus and kinetic evaluation was conducted by surface chemistry and Langmuir–Hinshelwood–Hougen–Watson (LHHW) type mode. Powder X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) were performed. Hydrogen adsorption capacity of commercial MgH{submore » 2}, milled MgH{sub 2}, and MgH{sub 2}/CNT composite are found to be 0.04, 0.057, and 0.059 g (H{sub 2})/g (MgH{sub 2}) at 673 K and hydrogen pressure of 4.6 MPa. Addition of 5 wt% of CNTs to MgH{sub 2} proved to be very critical to enhance hydrogen adsorption as well as to improve its kinetics. It was observed that hydrogen adsorption is not in quasi-state equilibrium and is modeled using kinetic rate laws.« less

Gram-scale production of B, N co-doped graphene-like carbon for high performance supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Chen, Zhuo; Hou, Liqiang; Cao, Yan; Tang, Yushu; Li, Yongfeng

2018-03-01

Boron and nitrogen co-doped graphene-like carbon (BNC) with a gram scale was synthesized via a two-step method including a ball-milling process and a calcination process and used as electrode materials for supercapacitors. High surface area and abundant active sites of graphene-like carbon were created by the ball-milling process. Interestingly, the nitrogen atoms are doped in carbon matrix without any other N sources except for air. The textual and chemical properties can be easily tuned by changing the calcination temperature, and at 900 oC the BNC with a high surface area (802.35 m2/g), a high boron content (2.19 at%), a hierarchical pore size distribution and a relatively high graphitic degree was obtained. It shows an excellent performance of high specific capacitance retention about 78.2% at high current density (199 F/g at 100 A/g) of the initial capacitance (254 F/g at 0.25 A/g) and good cycling stability (90% capacitance retention over 1000 cycles at 100 A/g) measured in a three-electrode system. Furthermore, in a two-electrode system, a specific capacitance of 225 F/g at 0.25 A/g and a good cycling stability (93% capacitance retention over 20,000 cycles at 25 A/g) were achieved by using BNC as electrodes. The strategy of synthesis is facile and effective to fabricate multi-doped graphene-like carbon for promising candidates as electrode materials in supercapacitors.

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

Effect of Sintering Temperature to Physical, Magnetic Properties and Crystal Structure on Permanent Magnet BaFe12O19 Prepared From Mill Scale

NASA Astrophysics Data System (ADS)

Ramlan; Muljadi; Sardjono, Priyo; Gulo, Fakhili; Setiabudidaya, Dedi

2017-07-01

Permanent magnet of Barium hexa Ferrite with formula BaFe12O19 has been made by metallurgy powder method from raw materials : Barium carbonate (BaCO3 E-merck) and Iron Oxide (Fe2O3 from mill scale). Both of raw materials have been mixed with stoichiometry composition by using a ball mill for 24 hours. The fine powder obtained from milling process was formed by using a hydraulic press at pressure 50 MPa and continued with sintering process. The sintering temperature was varied : 1150°C, 1200°C, 1250°C and 1300°C with holding time for 1 hour. The sintered samples were characterized such as : physical properties (bulk density, porosity and shrinkage), magnetic properties (flux density, remanence, coercivity and magnetic saturation) by using VSM and crystal structure by using XRD. According characterization results show that the crystal structure of BaFe12O19 does not change after sintering process, but the grain size tends to increase. The optimum condition is achieved at temperature 1250°C, and at this condition, the sample has characterization such as : bulk density = 4.35 g/cm3, porosity = 1.03% and firing shrinkage = 11.63%, flux density = 681.1 Gauss, remanence (σr) = 20.78 emu/g, coercivity (Hc) = 2058 Oe and magnetic saturation (σs) 45.16 emu/g.

Efficient removal of copper from wastewater by using mechanically activated calcium carbonate.

PubMed

Hu, Huimin; Li, Xuewei; Huang, Pengwu; Zhang, Qiwu; Yuan, Wenyi

2017-12-01

Copper removal from aqueous solution is necessary from the stances of both environmental protection and copper resource recycling. It is important to develop a new chemical precipitation method suitable for removing copper particularly at low concentration as the case of waste mine water, with regards to the various problems related to the current precipitation methods by using strong alkalis or soluble sulfides. In this research, we studied a possible chemical precipitation of copper ions at concentration around 60 mg/L or lower by cogrinding copper sulfate in water with calcium carbonate (CaCO 3 ) using wet stirred ball milling. With the aid of ball milling, copper precipitation as a basic sulfate (posnjakite: Cu 4 (SO 4 ) (OH) 6 ·H 2 O) occurred at a very high copper removal rate of 99.76%, to reduce the residual copper concentration in the solution less than 0.5 mg/L, reaching the discharge limit, even with the addition amount of CaCO 3 as a stoichiometric ratio of CaCO 3 /Cu 2+ at 1:1. It is more interesting to notice that, at the same conditions, other heavy metals such as Ni, Mn, Zn and Cd do not precipitate obviously just with CaCO 3 addition at CaCO 3 /M 2+ at 1:1 so that the precipitate without the impurities can be processed as good source to recover copper. This newly proposed concept can be further developed to treat wastewaters with other metals to serve both purposes of environmental purification and resource recovery in a similar way. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of metal matrix composites by powder metallurgy: A review

NASA Astrophysics Data System (ADS)

Manohar, Guttikonda; Dey, Abhijit; Pandey, K. M.; Maity, S. R.

2018-04-01

Now a day's metal matrix components are used in may industries and it finds the applications in many fields so, to make it as better performable materials. So, the need to increase the mechanical properties of the composites is there. As seen from previous studies major problem faced by the MMC's are wetting, interface bonding between reinforcement and matrix material while they are prepared by conventional methods like stir casting, squeeze casting and other techniques which uses liquid molten metals. So many researchers adopt PM to eliminate these defects and to increase the mechanical properties of the composites. Powder metallurgy is one of the better ways to prepare composites and Nano composites. And the major problem faced by the conventional methods are uniform distribution of the reinforcement particles in the matrix alloy, many researchers tried to homogeneously dispersion of reinforcements in matrix but they find it difficult through conventional methods, among all they find ultrasonic dispersion is efficient. This review article is mainly concentrated on importance of powder metallurgy in homogeneous distribution of reinforcement in matrix by ball milling or mechanical milling and how powder metallurgy improves the mechanical properties of the composites.

Rapid and direct synthesis of complex perovskite oxides through a highly energetic planetary milling

PubMed Central

Lee, Gyoung-Ja; Park, Eun-Kwang; Yang, Sun-A; Park, Jin-Ju; Bu, Sang-Don; Lee, Min-Ku

2017-01-01

The search for a new and facile synthetic route that is simple, economical and environmentally safe is one of the most challenging issues related to the synthesis of functional complex oxides. Herein, we report the expeditious synthesis of single-phase perovskite oxides by a high-rate mechanochemical reaction, which is generally difficult through conventional milling methods. With the help of a highly energetic planetary ball mill, lead-free piezoelectric perovskite oxides of (Bi, Na)TiO3, (K, Na)NbO3 and their modified complex compositions were directly synthesized with low contamination. The reaction time necessary to fully convert the micron-sized reactant powder mixture into a single-phase perovskite structure was markedly short at only 30–40 min regardless of the chemical composition. The cumulative kinetic energy required to overtake the activation period necessary for predominant formation of perovskite products was ca. 387 kJ/g for (Bi, Na)TiO3 and ca. 580 kJ/g for (K, Na)NbO3. The mechanochemically derived powders, when sintered, showed piezoelectric performance capabilities comparable to those of powders obtained by conventional solid-state reaction processes. The observed mechanochemical synthetic route may lead to the realization of a rapid, one-step preparation method by which to create other promising functional oxides without time-consuming homogenization and high-temperature calcination powder procedures. PMID:28387324

Observation of martensitic transformation in Ni50Mn41Cu4Sn5 Heusler alloy prepared by mechanical alloying

NASA Astrophysics Data System (ADS)

Saini, Dinesh; Singh, Satyavir; Banerjee, M. K.; Sachdev, K.

2017-05-01

Mechanical alloying route has been employed for preparation of a single phase Ni50Mn41Cu4Sn5 (atomic %) Heusler alloy. Use of high energy planetary ball mill enables successful preparation of the same as authenticated by detailed X-ray diffraction (XRD) study. Microstructural study is carried out by optical and scanning electron microscopic techniques. XRD results reveal that increasing milling time leads to reduction in crystallite size and concurrent increase in lattice strain. Microstructural results indicate formation of self-assembled martensite twins.

Processing-property relations in YBa2Cu3O(6+x) superconductors

NASA Astrophysics Data System (ADS)

Safari, A.; Wachtman, J. B., Jr.; Parkhe, V.; Caracciolo, R.; Jeter, D.

Processing of YBa2Cu3O(6+x) superconducting samples by employing different precursor powder preparation techniques such as ball milling, attrition milling, and narrow particle size distribution powder preparation through coprecipitation by spraying will be discussed. CuO coated with oxalates shows the lowest resistance above Tc up to room temperature. The extent of corrosion by water has been studied by employing magnetic susceptibility, XPS, and X-ray diffraction. Superconducting samples are affected to a considerable extent when treated in water at 60 C and the severity of the attack increases with time.

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

Quenching of reactive intermediates during mechanochemical depolymerization of lignin

DOE PAGES

Brittain, Alex D.; Chrisandina, Natasha J.; Cooper, Rachel E.; ...

2017-05-10

Mechanochemical reactions are performed to depolymerize organosolv lignin with sodium hydroxide in a mixer ball mill. GPC analysis reveals that rapid depolymerization into small oligomers occurs within minutes of milling time, followed by a slower reduction in average relative molecular mass over the next 8 h of milling. Monomeric products are identified by GC–MS and quantified by GC-FID. The extent of depolymerization appears to be limited by repolymerization reactions that form bonds between products. Suppression of these repolymerization reactions can be achieved through the addition of methanol as a scavenger or adjustment of the moisture content of the feedstock. Thesemore » modifications result in lower average relative molecular masses and higher yields of monomers. These results are an important step towards designing an efficient pathway for lignin valorization.« less

Magnetic properties of Ni nanoparticles dispersed in silica prepared by high-energy ball milling

NASA Astrophysics Data System (ADS)

González, E. M.; Montero, M. I.; Cebollada, F.; de Julián, C.; Vicent, J. L.; González, J. M.

1998-04-01

We analyze the magnetic properties of mechanically ground nanosized Ni particles dispersed in a SiO2 matrix. Our magnetic characterization of the as-milled samples show the occurrence of two blocking processes and that of non-monotonic milling time evolutions of the magnetic-order temperature, the high-field magnetization and the saturation coercivity. The measured coercivities exhibit giant values and a uniaxial-type temperature dependence. Thermal treatment carried out in the as-prepared samples result in a remarkable coercivity reduction and in an increase of the high-field magnetization. We conclude, on the basis of the consideration of a core (pure Ni) and shell (Ni-Si inhomogeneous alloy) particle structure, that the magnetoelastic anisotropy plays the dominant role in determining the magnetic properties of our particles.

Ceramic fiber-reinforced monoclinic celsian phase glass-ceramic matrix composite material

NASA Technical Reports Server (NTRS)

Bansal, Narottam P. (Inventor); Dicarlo, James A. (Inventor)

1994-01-01

A hyridopolysilazane-derived ceramic fiber reinforced monoclinic celsian phase barium aluminum silicate glass-ceramic matrix composite material is prepared by ball-milling an aqueous slurry of BAS glass powder and fine monoclinic celsian seeds. The fibers improve the mechanical strength and fracture toughness and with the matrix provide superior dielectric properties.

Magnetic strength and corrosion of rare earth magnets.

PubMed

Ahmad, Khalid A; Drummond, James L; Graber, Thomas; BeGole, Ellen

2006-09-01

Rare earth magnets have been used in orthodontics, but their corrosion tendency in the oral cavity limits long-term clinical application. The aim of this project was to evaluate several; magnet coatings and their effects on magnetic flux density. A total of 60 neodymium-iron-boron magnets divided into 6 equal groups--polytetrafluoroethylene-coated (PTFE), parylene-coated, and noncoated--were subjected to 4 weeks of aging in saline solution, ball milling, and corrosion testing. A significant decrease in magnet flux density was recorded after applying a protective layer of parylene, whereas a slight decrease was found after applying a protective layer of PTFE. After 4 weeks of aging, the coated magnets were superior to the noncoated magnets in retaining magnetism. The corrosion-behavior test showed no significant difference between the 2 types of coated magnets, and considerable amounts of iron-leached ions were seen in all groups. Throughout the processes of coating, soaking, ball milling, and corrosion testing, PTFE was a better coating material than parylene for preserving magnet flux density. However, corrosion testing showed significant metal leaching in all groups.

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.

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

Grain boundary character distribution in nanocrystalline metals produced by different processing routes

DOE PAGES

Bober, David B.; Kumar, Mukal; Rupert, Timothy J.; ...

2015-12-28

Nanocrystalline materials are defined by their fine grain size, but details of the grain boundary character distribution should also be important. Grain boundary character distributions are reported for ball-milled, sputter-deposited, and electrodeposited Ni and Ni-based alloys, all with average grain sizes of ~20 nm, to study the influence of processing route. The two deposited materials had nearly identical grain boundary character distributions, both marked by a Σ3 length percentage of 23 to 25 pct. In contrast, the ball-milled material had only 3 pct Σ3-type grain boundaries and a large fraction of low-angle boundaries (16 pct), with the remainder being predominantlymore » random high angle (73 pct). Furthermore, these grain boundary character measurements are connected to the physical events that control their respective processing routes. Consequences for material properties are also discussed with a focus on nanocrystalline corrosion. As a whole, the results presented here show that grain boundary character distribution, which has often been overlooked in nanocrystalline metals, can vary significantly and influence material properties in profound ways.« less

Electrical conductivity and magnetic field dependent current-voltage characteristics of nanocrystalline nickel ferrite

NASA Astrophysics Data System (ADS)

Ghosh, P.; Bhowmik, R. N.; Das, M. R.; Mitra, P.

2017-04-01

We have studied the grain size dependent electrical conductivity, dielectric relaxation and magnetic field dependent current voltage (I - V) characteristics of nickel ferrite (NiFe2O4) . The material has been synthesized by sol-gel self-combustion technique, followed by ball milling at room temperature in air environment to control the grain size. The material has been characterized using X-ray diffraction (refined with MAUD software analysis) and Transmission electron microscopy. Impedance spectroscopy and I - V characteristics in the presence of variable magnetic fields have confirmed the increase of resistivity for the fine powdered samples (grain size 5.17±0.6 nm), resulted from ball milling of the chemical routed sample. Activation energy of the material for electrical charge hopping process has increased with the decrease of grain size by mechanical milling of chemical routed sample. The I - V curves showed many highly non-linear and irreversible electrical features, e.g., I - V loop and bi-stable electronic states (low resistance state-LRS and high resistance state-HRS) on cycling the electrical bias voltage direction during I-V curve measurement. The electrical dc resistance for the chemically routed (without milled) sample in HRS (∼3.4876×104 Ω) at 20 V in presence of magnetic field 10 kOe has enhanced to ∼3.4152×105 Ω for the 10 h milled sample. The samples exhibited an unusual negative differential resistance (NDR) effect that gradually decreased on decreasing the grain size of the material. The magneto-resistance of the samples at room temperature has been found substantially large (∼25-65%). The control of electrical charge transport properties under magnetic field, as observed in the present ferrimagnetic material, indicate the magneto-electric coupling in the materials and the results could be useful in spintronics applications.

Properties of plate-like carbonyl iron particle for magnetorheological fluid

NASA Astrophysics Data System (ADS)

Shilan, S. T.; Mazlan, S. A.; Khairi, M. H. A.; Ubaidillah

2016-11-01

This work experimentally discussed the characterization, magnetic, and rheological properties of plate-like carbonyl iron particle (CIP) in comparison with conventional spherical CIP. Plate-like CIP was produced by using ball milling method. The effect of plate-like shape on the magnetic behavior of CIP was firstly investigated by vibrating sample magnetometer (VSM). The results indicated that the plate-like CIP obtained higher saturation magnetization (about 8%) than that of the spherical particles. In addition, the field-dependent rheological properties such as yield stress were investigated and the results are compared between two particles as a function of the magnetic field intensity.

Observation of ferromagnetism in Mn doped KNbO3

NASA Astrophysics Data System (ADS)

Manikandan, M.; Venkateswaran, C.

2015-06-01

Pure and Mn doped KNbO3 have been prepared by ball milling assisted ceramic method. Mn ion had been doped at Nb site to induce ferromagnetism at room temperature. X-ray diffraction (XRD) patterns reveal the formation of orthorhombic phase. High resolution scanning electron micrograph (HR-SEM) of both pure and Mn doped samples show a mixture of spherical and plate like particles. Room temperature magnetic behavior of both the samples were analyzed using vibrating sample magnetometer (VSM). 5% Mn doped KNbO3 exhibits ferromagnetic behavior. Observed ferromagnetic feature has been explained by interactions between bound magnetic polarons which are created by Mn4+ ions.

Characterization of nanodimensional Ni-Zn ferrite prepared by mechanochemical and thermal methods

NASA Astrophysics Data System (ADS)

Manova, E.; Paneva, D.; Kunev, B.; Rivière, E.; Estournès, C.; Mitov, I.

2010-03-01

Nickel zinc ferrite nanoparticles, Ni1-xZnxFe2O4 (x = 0, 0.2, 0.5, 0.8, 1.0), with dimensions below 10 nm have been prepared by combining chemical precipitation with high-energy ball milling. For comparison, their analogues obtained by thermal synthesis have also been studied. Mössbauer spectroscopy, X-ray diffraction, and magnetic measurements are used for the characterization of the obtained materials. X-ray diffraction shows that after 3h of mechanical treatment ferrites containing zinc are formed, while 6h of treatment is needed to obtain NiFe2O4. The magnetic properties of the samples exhibit a strong dependence on the phase composition, particle size and preparation method.

cathode material for Li-ion batteries

NASA Astrophysics Data System (ADS)

Wang, Yanming; Wang, Yajing; Wang, Fei

2014-05-01

Well-crystallized Li2NiTiO4 nanoparticles are rapidly synthesized by a molten salt method using a mixture of NaCl and KCl salts. X-ray diffraction pattern and scanning electron microscopic image show that Li2NiTiO4 has a cubic rock salt structure with an average particle size of ca. 50 nm. Conductive carbon-coated Li2NiTiO4 is obtained by a facile ball milling method. As a novel 4 V positive cathode material for Li-ion batteries, the Li2NiTiO4/C delivers high discharge capacities of 115 mAh g-1 at room temperature and 138 mAh g-1 and 50°C, along with a superior cyclability.

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.

Synthesis and Explosive Consolidation of Titanium, Aluminium, Boron and Carbon Containing Powders

NASA Astrophysics Data System (ADS)

Chikhradze, Mikheil; Oniashvili, George; Chikhradze, Nikoloz; D. S Marquis, Fernand

2016-10-01

The development of modern technologies in the field of materials science has increased the interest towards the bulk materials with improved physical, chemical and mechanical properties. Composites, fabricated in Ti-Al-B-C systems are characterized by unique physical and mechanical properties. They are attractive for aerospace, power engineering, machine and chemical applications. The technologies to fabricate ultrafine grained powder and bulk materials in Ti-Al-B-C system are described in the paper. It includes results of theoretical and experimental investigation for selection of powders composition and determination of thermodynamic conditions for bland preparation, as well as optimal technological parameters for mechanical alloying and adiabatic compaction. The crystalline coarse Ti, Al, C powders and amorphous B were used as precursors and blends with different compositions of Ti-Al, Ti-Al-C, Ti-B-C and Ti-Al-B were prepared. Preliminary determination/selection of blend compositions was made on the basis of phase diagrams. The powders were mixed according to the selected ratios of components to produce the blend. Blends were processed in “Fritsch” Planetary premium line ball mill for mechanical alloying, syntheses of new phases, amorphization and ultrafine powder production. The blends processing time was variable: 1 to 20 hours. The optimal technological regimes of nano blend preparation were determined experimentally. Ball milled nano blends were placed in metallic tube and loaded by shock waves for realization of consolidation in adiabatic regime. The structure and properties of the obtained ultrafine grained materials depending on the processing parameters are investigated and discussed. For consolidation of the mixture, explosive compaction technology is applied at room temperatures. The prepared mixtures were located in low carbon steel tube and blast energies were used for explosive consolidation compositions. The relationship of ball milling technological parameters and explosive consolidation conditions on the structure/properties of the obtained samples are described in the paper.

Influence of excipients in comilling on mitigating milling-induced amorphization or structural disorder of crystalline pharmaceutical actives.

PubMed

Balani, Prashant N; Ng, Wai Kiong; Tan, Reginald B H; Chan, Sui Yung

2010-05-01

The feasibility of using excipients to suppress the amorphization or structural disorder of crystalline salbutamol sulphate (SS) during milling was investigated. SS was subjected to ball-milling in the presence of alpha-lactose monohydrate (LAC), adipic acid (AA), magnesium stearate (MgSt), or polyvinyl pyrrolidone (PVP). X-ray powder diffraction, dynamic vapor sorption (DVS), high sensitivity differential scanning calorimetry (HSDSC) were used to analyze the crystallinity of the milled mixtures. Comilling with crystalline excipients, LAC, AA, and MgSt proved effective in reducing the amorphization of SS. LAC, AA, or MgSt acting as seed crystals to induce recrystallization of amorphous SS formed by milling. During comilling, both SS and LAC turned predominantly amorphous after 45 min but transformed back to a highly crystalline state after 60 min. Amorphous content was below the detection limits of DVS (0.5%) and HSDSC (5%). Comilled and physical mixtures of SS and ALM were stored under normal and elevated humidity conditions. This was found to prevent subsequent changes in crystallinity and morphology of comilled SS:LAC as compared to significant changes in milled SS and physical mixture. These results demonstrate a promising application of comilling with crystalline excipients in mitigating milling induced amorphization of pharmaceutical actives.

Improved Method Being Developed for Surface Enhancement of Metallic Materials

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Telesman, Jack; Kantzos, Peter T.

2001-01-01

Surface enhancement methods induce a layer of beneficial residual compressive stress to improve the impact (FOD) resistance and fatigue life of metallic materials. A traditional method of surface enhancement often used is shot peening, in which small steel spheres are repeatedly impinged on metallic surfaces. Shot peening is inexpensive and widely used, but the plastic deformation of 20 to 40 percent imparted by the impacts can be harmful. This plastic deformation can damage the microstructure, severely limiting the ductility and durability of the material near the surface. It has also been shown to promote accelerated relaxation of the beneficial compressive residual stresses at elevated temperatures. Low-plasticity burnishing (LPB) is being developed as an improved method for the surface enhancement of metallic materials. LPB is being investigated as a rapid, inexpensive surface enhancement method under NASA Small Business Innovation Research contracts NAS3-98034 and NAS3-99116, with supporting characterization work at NASA. Previously, roller burnishing had been employed to refine surface finish. This concept was adopted and then optimized as a means of producing a layer of compressive stress of high magnitude and depth, with minimal plastic deformation (ref. 1). A simplified diagram of the developed process is given in the following figure. A single pass of a smooth, free-rolling spherical ball under a normal force deforms the surface of the material in tension, creating a compressive layer of residual stress. The ball is supported in a fluid with sufficient pressure to lift the ball off the surface of the retaining spherical socket. The ball is only in mechanical contact with the surface of the material being burnished and is free to roll on the surface. This apparatus is designed to be mounted in the conventional lathes and vertical mills currently used to machine parts. The process has been successfully applied to nickel-base superalloys by a team from the NASA Glenn Research Center, Lambda Research, and METCUT Research, as supported by the NASA Small Business Innovation Research Phase I and II programs, the Ultra Safe program, and the Ultra- Efficient Engine Technology (UEET) Program.

Defect engineered oxides for enhanced mechanochemical destruction of halogenated organic pollutants.

PubMed

Cagnetta, Giovanni; Huang, Jun; Lu, Mengnan; Wang, Bin; Wang, Yujue; Deng, Shubo; Yu, Gang

2017-10-01

Mechanochemical activation of metal oxides is studied by a novel methodology based on solid state reaction with a stable radical specie. Such approach corroborates that vacancy formation by high energy ball milling, also in nonreducible oxides, is responsible for electron release on particles' surfaces. This finding suggests a new defect engineering strategy to improve effectiveness of metal oxides as co-milling reagent for halogenated organic pollutant destruction. Results prove that high valent metal doping of a commonly employed co-milling reagent such as CaO determines 2.5 times faster pollutant degradation rate. This enhancement is due to electron-rich defects generated by the dopant; electrons are transferred to the organic pollutant thus causing its mineralization. The proposed strategy can be easily applied to other reagents. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Selamat, Mohd Zulkefli, E-mail: azulkeflis@utem.edu.my; Yusuf, Muhammad Yusri Md, E-mail: yusri.cheras@gmail.com; Wer, Tio Kok, E-mail: to91@hotmail.my

Bipolar plates are key components in Proton Exchange Membrane (PEM) fuel cells. They carry current away from the cell and withstand the clamping force of the stack assembly. Therefore, PEM fuel cell bipolar plates must have high electrical conductivity and adequate mechanical strength, in addition to being light weight and low cost in terms of both applicable materials and production methods. In this research, the raw materials used to fabricate the high performance bipolar plate are Graphite (Gr), Stannum (Sn) and Polypropylene (PP). All materials used was in powder form and Gr and Sn act as fillers and the PPmore » acts as binder. The ratio of fillers (Gr/Sn) and binder (PP) was fixed at 80:20. For the multi-conductive filler, small amount of Sn, which is 10 up to 20wt% (from the total weight of fillers 80%) have been added into Gr/Sn/PP composite. The fillers were mixed by using the ball mill machine. The second stage of mixing process between the mixer of fillers and binder is also carried out by using ball mill machine before the compaction process by the hot press machine. The effect of formation temperatures (160°C-170°C) on the properties of Gr/Sn/PP composite had been studied in detail, especially the electrical conductivity, bulk density, hardness and microstructure analysis of Gr/Sn/PP composite. The result shows that there are significant improvement in the electrical conductivity and bulk density, which are exceeding the US-DoE target with the maximum value of 265.35 S/cm and 1.682g/cm{sup 3} respectively.« 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

Electrochemical performance of NCM/LFP/Al composite cathode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Allahyari, Ehsan; Ghorbanzadeh, Milad; Riahifar, Reza; Hadavi, S. M. M.

2018-05-01

The LiNi0.5Mn0.3Co0.2O2 (NCM) was synthesized via conventional solution combustion synthesis method. Different amounts of LiFePO4 (10, 20 and 30 wt%) were added to NCM via the ball milling technique to improve electrochemical performance including discharge capacity, cycle stability, and rate capability. The LiNi0.5Mn0.3Co0.2O2/LiFePO4 containing 20 wt% LiFePO4 was considered as the optimum composition according to the electrochemical results and SEM images. The Al powder was added to optimum LiNi0.5Mn0.3Co0.2/LiFePO4-0.2 composite through planetary ball mill to enhance the conductivity of LiNi0.5Mn0.3Co0.2O2/LiFePO4-0.2. The LiNi0.5Mn0.3Co0.2O2/LiFePO4-0.2/Al composite cathodes provide better electrochemical performance compared to pure LiNi0.5Mn0.3Co0.2O2 cathodes. The results indicate that by addition of 20 wt% of LiFePO4, the internal resistance of the electrode as well as the charge transfer resistance are reduced. Due to the strong P–O bond of the PO4 in LiFePO4, side reactions between the active electrode and electrolyte is prevented. In addition, according to weakness of the Ionic conductivity in solid electrolyte, in this paper aluminum powders added to the electrode for resolving this problem.

Enzymatic hydrolysis of loblolly pine: effects of cellulose crystallinity and delignification

Treesearch

Umesh P. Agarwal; J.Y. Zhu; Sally A. Ralph

2013-01-01

Hydrolysis experiments with commercial cellulases have been performed to understand the effects of cell wall crystallinity and lignin on the process. In the focus of the paper are loblolly pine wood samples, which were systematically delignified and partly ball-milled, and, for comparison, Whatman CC31 cellulose samples with different crystallinities. In pure cellulose...

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.

Study on the Classification of the Uranium Mineral of Venta de Cardena; ESTUDIO SOBRE LA CLASIFICACION DEL MINERAL DE VENTA DE CARDENA

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

Otero, A.R.

1959-01-01

The behavior of uranium mineral from Venta de Cardena in a spiral classifier which operates in a closed system with a ball mill was studied to obtain data for the design of a milling-classification system with a production capacity of 200 tons per day with a particle size less than 0.417 mm. The characteristics of such a system, the problems in normal operation, the inconveriences which these cause, and their solution were investigated. Correlations between these tests and the results obtained with long glass tubes are presented. (J.S.R.)

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.

Mechanochemical Phosphorylation and Solubilisation of β-D-Glucan from Yeast Saccharomyces cerevisiae and Its Biological Activities

PubMed Central

Shi, Feng; Shi, Jikui; Li, Yongfu

2014-01-01

To obtain a water-soluble β-D-glucan derivative cleanly and conveniently, a highly efficient mechanochemical method, planetary ball milling, was used to phosphorylate β-D-glucan isolated from yeast Saccharomyces cerevisiae in solid state. Soluble β-D-glucan phosphate (GP) with a high degree of substitution (0.77–2.09) and an apparent PEAK molecular weight of 6.6–10.0 kDa was produced when β-D-glucan was co-milled with sodium hexametaphosphate at 139.5–186.0 rad/s for 12–20 min. The energy transferred was 3.03–11.98 KJ/g. The phosphorylation of GPs was demonstrated by Fourier transform infrared spectroscopy and 13C and 31P Nuclear magnetic resonance spectroscopy. Three GP products with different degree of substitution (DS) and degree of polymerisation (DP) were able to upregulate the functional events mediated by activated murine macrophage RAW264.7 cells, among which GP-2 with a DS of 1.24 and DP of 30.5 exerted the highest immunostimulating activity. Our results indicate that mechanochemical processing is an efficient method for preparing water-soluble and biologically active GP with high DS. PMID:25075740

Effect of synthesizing method on the properties of LiFePO4/C composite for rechargeable lithium-ion batteries

NASA Astrophysics Data System (ADS)

Yoon, Man-Soon; Islam, Mobinul; Park, Young Min; Ur, Soon-Chul

2013-03-01

Olivine-type LiFePO4/C cathode materials are fabricated with FePO4 powders that are pre-synthesized by two different processes from iron chloride solution. Process I is a modified precipitation method which is implemented by the pH control of a solution using NH4OH to form FePO4 precipitates at room temperature. Process II is a conventional precipitation method, of which H3PO4 (85%) solution is gradually added to a FeCl3 solution during the process to maintain a designated mole ratio. The solution is subsequently aged at 90°C in a water bath until FePO4 precipitates appear. In order to synthesize LiFePO4/C composites, each batch of FePO4 powders is then mixed with pre-milled lithium carbonate and glucose (8 wt. %) as a carbon source in a ball-mill. The structural characteristics of both LiFePO4/C composites fabricated using iron phospates from two different routes have been examined employing XRD and SEM. The modified precipitation process is considered to be a relatively simple and effective process for the preparation of LiFePO4/C composites owing to their excellent electrochemical properties and rate capabilities.

Facile molten salt synthesis of Li2NiTiO4 cathode material for Li-ion batteries.

PubMed

Wang, Yanming; Wang, Yajing; Wang, Fei

2014-01-01

Well-crystallized Li2NiTiO4 nanoparticles are rapidly synthesized by a molten salt method using a mixture of NaCl and KCl salts. X-ray diffraction pattern and scanning electron microscopic image show that Li2NiTiO4 has a cubic rock salt structure with an average particle size of ca. 50 nm. Conductive carbon-coated Li2NiTiO4 is obtained by a facile ball milling method. As a novel 4 V positive cathode material for Li-ion batteries, the Li2NiTiO4/C delivers high discharge capacities of 115 mAh g(-1) at room temperature and 138 mAh g(-1) and 50°C, along with a superior cyclability.

Solid State Reduction of MoO3 with Carbon via Mechanical Alloying to Synthesize Nano-Crystaline MoO2

NASA Astrophysics Data System (ADS)

Saghafi, M.; Ataie, A.; Heshmati-Manesh, S.

In this research, effect of milling time on solid state reduction of MoO3 with carbon has been investigated. It was found that mechanical activation of a mixture of MoO3 and carbon at ambient temperature by high energy ball milling was not able to reduce MoO3 to metallic molybdenum. MoO3 was converted to MoO2 at the first stage of reduction and peaks of the latter phase in X-ray diffraction patterns were detected when the milling time exceeded from 50 hours. The main effect of increased milling time at this stage was decreasing of MoO3 peak intensities and significant peak broadening due to decrease in size of crystallites. After prolonged milling, MoO3 was fully reduced to nano-crystalline MoO2 and its mean crystallite size was calculated using Williamson-Hall technique and found to be 17.5 nm. Thermodynamic investigations also confirm the possibility of reduction of MoO3 to MoO2 during the milling operation at room temperature. But, further reduction to metallic molybdenum requires thermal activation at higher temperature near 1100 K. XRD and SEM techniques were employed to evaluate the powder particles characteristics.

Structural and magnetic studies of half-metallic Heusler alloy Cr2CoSi nanoparticle synthesized by mechanical-alloying method

NASA Astrophysics Data System (ADS)

Saravanan, G.; Asvini, V.; Kalaiezhily, R. K.; Ravichandran, K.

2018-05-01

Heusler Alloy based Cr2CoSi nanoparticles were synthesized by using ball milling. X-ray diffractions studies were used to characterize the crystal structure of Cr2CoSi nanoparticles and magnetic properties were studied using VSM. XRD data analysis confirms the Heusler alloy phase showing the L21 structure. Magnetic properties are measured for synthesized samples having coercivity Hc = 389 Oe, with high saturation magnetization value Ms = 8.64 emu/g and remenance value Mr = 2.93 emu/g. Synthesized Heusler alloy Cr2CoSi nanoparticles can be potential materials for use in Spin polarized based spin sensors, spin devices, magnetic sensors and transducer applications.

Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

PubMed

Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

2016-02-01

Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

TECHNICAL NOTE: The effect of the green additive guar gum on the properties of magnetorheological fluid

NASA Astrophysics Data System (ADS)

Fang, Chen; Zhao, Bin Yuan; Chen, LeSheng; Wu, Qing; Liu, Nan; Hu, Ke Ao

2005-02-01

Magnetorheological (MR) fluid containing guar gum was prepared for the first time by ball-milling the guar gum powder together with silicone oil and carbonyl iron powder. By forming a coating layer over the ground carbonyl iron powder, the guar gum improves the sedimentation stability and thixotropy of the MR fluid effectively.

Electrodeposited Nanostructured Films and Coatings: Synthesis, Structure, Properties and Applications

DTIC Science & Technology

2000-01-01

function of the Electrodeposited Layer Thickness", B.Sc Thesis , Queen’s University, Kingston, Ontario, Canada 34) Merchant, H. K., (1995) in "Defect...The following component part numbers comprise the compilation report: ADPO11800 thru ADP011832 UNCLASSIFIED ELECTRODEPOSITED NANOSTRUCTURED FILMS AND...thermomechanical processing, ball milling, rapid solidification, electrodeposition ), unique material performance characteristics in bulk materials as well as

DETAIL OVERHEAD VIEW OF SECONDARY ORE BIN. CONVEYOR PLATFORM,TRAM TRESTLE, ...

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

DETAIL OVERHEAD VIEW OF SECONDARY ORE BIN. CONVEYOR PLATFORM,TRAM TRESTLE, AND LOADING PLATFORM. LOOKING SOUTHWEST. THE HOLE IN THE ORE BIN FLOOR CAN BE SEEN, AND BALL MILL FOUNDATION AT LOWER LEFT CORNER. SEE CA-291-47(CT) FOR IDENTICAL COLOR TRANSPARENCY. - Keane Wonder Mine, Park Route 4 (Daylight Pass Cutoff), Death Valley Junction, Inyo County, CA

DETAIL OVERHEAD VIEW OF SECONDARY ORE BIN, CONVEYOR PLATFORM TRAM ...

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

DETAIL OVERHEAD VIEW OF SECONDARY ORE BIN, CONVEYOR PLATFORM TRAM TRESTLE, AND LOADING PLATFORM, LOOKING SOUTHWEST. THE HOLE IN THE ORE BIN FLOOR CAN BE SEEN, AND BALL MILL FOUNDATION AT LOWER LEFT CORNER. SEE CA-291-13 FOR IDENTICAL B&W NEGATIVE. - Keane Wonder Mine, Park Route 4 (Daylight Pass Cutoff), Death Valley Junction, Inyo County, CA

Ball-free mechanochemistry: in situ real-time monitoring of pharmaceutical co-crystal formation by resonant acoustic mixing.

PubMed

Michalchuk, Adam A L; Hope, Karl S; Kennedy, Stuart R; Blanco, Maria V; Boldyreva, Elena V; Pulham, Colin R

2018-04-17

Resonant acoustic mixing (RAM) is a new technology designed for intensive mixing of powders that offers the capability to process powders with minimal damage to particles. This feature is particularly important for mixing impact-sensitive materials such as explosives and propellants. While the RAM technique has been extensively employed for the mixing of powders and viscous polymers, comparatively little is known about its use for mechanosynthesis. We present here the first in situ study of RAM-induced co-crystallisation monitored using synchrotron X-ray powder diffraction. The phase profile of the reaction between nicotinamide and carbamazepine in the presence of a small amount of water was monitored at two different relative accelerations of the mixer. In marked contrast to ball-milling techniques, the lack of milling bodies in the RAM experiment does not hinder co-crystallisation of the two starting materials, which occurred readily and was independent of the frequency of oscillation. The reaction could be optimised by enhancing the number of reactive contacts through mixing and comminution. These observations provide new insight into the role of various experimental parameters in conventional mechanochemistry using liquid-assisted grinding techniques.

Direct ethanol production from starch, wheat bran and rice straw by the white rot fungus Trametes hirsuta.

PubMed

Okamoto, Kenji; Nitta, Yasuyuki; Maekawa, Nitaro; Yanase, Hideshi

2011-03-07

The white rot fungus Trametes hirsuta produced ethanol from a variety of hexoses: glucose, mannose, cellobiose and maltose, with yields of 0.49, 0.48, 0.47 and 0.47 g/g of ethanol per sugar utilized, respectively. In addition, this fungus showed relatively favorable xylose consumption and ethanol production with a yield of 0.44 g/g. T. hirsuta was capable of directly fermenting starch, wheat bran and rice straw to ethanol without acid or enzymatic hydrolysis. Maximum ethanol concentrations of 9.1, 4.3 and 3.0 g/l, corresponding to 89.2%, 78.8% and 57.4% of the theoretical yield, were obtained when the fungus was grown in a medium containing 20 g/l starch, wheat bran or rice straw, respectively. The fermentation of rice straw pretreated with ball milling led to a small improvement in the ethanol yield: 3.4 g ethanol/20 g ball-milled rice straw. As T. hirsuta is an efficient microorganism capable of hydrolyzing biomass to fermentable sugars and directly converting them to ethanol, it may represent a suitable microorganism in consolidated bioprocessing applications. Copyright © 2010 Elsevier Inc. All rights reserved.

Solid state consolidation nanocrystalline copper-tungsten using cold spray

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

Hall, Aaron Christopher; Sarobol, Pylin; Argibay, Nicolas

It is well known that nanostructured metals can exhibit significantly improved properties compared to metals with conventional grain size. Unfortunately, nanocrystalline metals typically are not thermodynamically stable and exhibit rapid grain growth at moderate temperatures. This severely limits their processing and use, making them impractical for most engineering applications. Recent work has shown that a number of thermodynamically stable nanocrystalline metal alloys exist. These alloys have been prepared as powders using severe plastic deformation (e.g. ball milling) processes. Consolidation of these powders without compromise of their nanocrystalline microstructure is a critical step to enabling their use as engineering materials. Wemore » demonstrate solid-state consolidation of ball milled copper-tantalum nanocrystalline metal powder using cold spray. Unfortunately, the nanocrystalline copper-tantalum powder that was consolidated did not contain the thermodynamically stable copper-tantalum nanostructure. Nevertheless, this does this demonstrates a pathway to preparation of bulk thermodynamically stable nanocrystalline copper-tantalum. Furthermore, it demonstrates a pathway to additive manufacturing (3D printing) of nanocrystalline copper-tantalum. Additive manufacturing of thermodynamically stable nanocrystalline metals is attractive because it enables maximum flexibility and efficiency in the use of these unique materials.« less

A green and efficient technology for the degradation of cellulosic materials: structure changes and enhanced enzymatic hydrolysis of natural cellulose pretreated by synergistic interaction of mechanical activation and metal salt.

PubMed

Zhang, Yanjuan; Li, Qian; Su, Jianmei; Lin, Ye; Huang, Zuqiang; Lu, Yinghua; Sun, Guosong; Yang, Mei; Huang, Aimin; Hu, Huayu; Zhu, Yuanqin

2015-02-01

A new technology for the pretreatment of natural cellulose was developed, which combined mechanical activation (MA) and metal salt treatments in a stirring ball mill. Different valent metal nitrates were used to investigate the changes in degree of polymerization (DP) and crystallinity index (CrI) of cellulose after MA+metal salt (MAMS) pretreatment, and Al(NO3)3 showed better pretreatment effect than NaNO3 and Zn(NO3)2. The destruction of morphological structure of cellulose was mainly resulted from intense ball milling, and the comparative studies on the changes of DP and crystal structure of MA and MA+Al(NO3)3 pretreated cellulose samples showed a synergistic interaction of MA and Al(NO3)3 treatments with more effective changes of structural characteristics of MA+Al(NO3)3 pretreated cellulose and substantial increase of reducing sugar yield in enzymatic hydrolysis of cellulose. In addition, the results indicated that the presence of Al(NO3)3 had significant enhancement for the enzymatic hydrolysis of cellulose. Copyright © 2014 Elsevier Ltd. All rights reserved.

Insights on the fundamental lithium storage behavior of all-solid-state lithium batteries containing the LiNi0.8Co0.15Al0.05O2 cathode and sulfide electrolyte

NASA Astrophysics Data System (ADS)

Peng, Gang; Yao, Xiayin; Wan, Hongli; Huang, Bingxin; Yin, Jingyun; Ding, Fei; Xu, Xiaoxiong

2016-03-01

An insightful study on the fundamental lithium storage behavior of all-solid-state lithium battery with a structure of LiNi0.8Co0.15Al0.05O2 (NCA)/Li10GeP2S12/Li-In is carried out in this work. The relationship between electrochemical performances and particle size, surface impurities and defects of the NCA positive material is systematically investigated. It is found that a ball-milling technique can decrease the particle size and remove surface impurities of the NCA cathode while also give rise to surface defects which could be recovered by a post-annealing process. The results indicate that the interfacial resistance between the NCA and Li10GeP2S12 is obviously decreased during the ball-milling followed by a post-annealing. Consequently, the discharge capacity of NCA in the NCA/Li10GeP2S12/Li-In solid-state battery is significantly enhanced, which exhibits a discharge capacity of 146 mAh g-1 at 25 °C.

Novel biochar-impregnated calcium alginate beads with improved water holding and nutrient retention properties.

PubMed

Wang, Bing; Gao, Bin; Zimmerman, Andrew R; Zheng, Yulin; Lyu, Honghong

2018-03-01

Drought conditions and nutrients loss have serious impacts on soil quality as well as crop yields in agroecosystems. New techniques are needed to carry out effective soil water and nutrient conservation and fertilizer application tools. Here, calcium alginate (CA) beads impregnated with ball-milled biochar (BMB) were investigated as a new type of water/nutrients retention agent. Both CA and Ca-alginate/ball milled biochar composite (CA-BMB) beads showed high kinetic swelling ratios in KNO 3 solution and low kinetic swelling ratios in water, indicating that CA-BMB beads have the potential to retain mineral nitrogen and nutrients by ion exchange. Pseudo-second-order kinetic model well-described the swelling kinetics of both beads in KNO 3 solution. Over a range of temperatures, the characteristics of dehydration suggested that impregnation with BMB improved the water holding capacity and postponed the dehydration time of Ca-alginate. The cumulative swelling and release characteristics of water, K + , and NO 3 - indicated that CA-BMB beads have great potential as a soil amendment to improve its nutrient retention and water holding capacity. Copyright © 2017 Elsevier Ltd. All rights reserved.

Flapper Valve and Hayfork: Functional anatomy and taxonomic potential of the Gastric Mill of Bairdioidea (Ostracoda, Podocopida).

PubMed

Maddocks, Rosalie F

2018-02-07

The chewing apparatus of the Bairdioidea has been described just once and is rarely illustrated, but it might have more taxonomic significance than commonly supposed. It is constructed as a flapper valve (hinged check valve), which is unique among Ostracoda and unusual among animals. It projects into the midgut and is substantially enveloped by it. It serves three functions: to move bites of food into the stomach, to close the esophagus against back-flow, and to pack strands of food and mucus onto the rotating food ball. It is probably less effective for macerating the food to reduce particle size. Two braces anchor this structure to the lateral wall of the forehead. It is lined by cuticle that is shed at each molt, and the formation of food balls is interrupted during molting. In its construction and action, this apparatus is quite unlike the gastric mill of decapod crustaceans, and it shows only distant homology to the dorsal Wulst of Cypridoidea. Some architectural details differ among families and genera. The well-sclerotized plate has some potential for fossil preservation in exceptional circumstances. A revised anatomical analysis is presented, together with an annotated glossary of terms.

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.

Magnetic properties of NdFeB-coated rubberwood composites

NASA Astrophysics Data System (ADS)

Noodam, Jureeporn; Sirisathitkul, Chitnarong; Matan, Nirundorn; Rattanasakulthong, Watcharee; Jantaratana, Pongsakorn

2013-01-01

Magnetic properties of composites prepared by coating lacquer containing neodymium iron boron (Nd-Fe-B) powders on rubberwood were characterized by vibrating sample magnetometry (VSM), magnetic moment measurements, and attraction tests with an iron-core solenoid. The Nd-Fe-B powders were recycled from electronic wastes by the ball-milling technique. Varying the milling time from 20 to 300 min, the magnetic squareness and the coercive field of the Nd-Fe-B powders were at the minimum when the powders were milled for 130 min. It followed that the coercive field of the magnetic wood composites was increased with the milling time increasing from 130 to 300 min. For the magnetic wood composites using Nd-Fe-B obtained from the same milling time, the magnetic squareness and the coercive field were rather insensitive to the variation of Nd-Fe-B concentration in coating lacquer from 0.43 to 1.00 g/cm3. By contrast, the magnetization and magnetic moment were increased with the Nd-Fe-B concentration increasing. Furthermore, the electrical current in the solenoid required for the attraction of the magnetic wood composites was exponentially reduced with the increase in the amount of Nd-Fe-B used in the coating.

Characterization of water based nanofluid for quench medium

NASA Astrophysics Data System (ADS)

Kresnodrianto; Harjanto, S.; Putra, W. N.; Ramahdita, G.; Yahya, S. S.; Mahiswara, E. P.

2018-04-01

Quenching has been a valuable method in steel hardening method especially in industrial scale. The hardenability of the metal alloys, the thickness of the component, and the geometry is some factors that can affect the choice of quench medium. Improper quench media can cause the material to become too brittle, suffers some geometric distortion, and undesirable residual stress that will cause some effect on the mechanical property and fracture mechanism of a component. Recently, nanofluid as a quench medium has been used for better quenching performance and has been studied using several different fluids and nanoparticles. Some of frequently used solvents include polymers, vegetable oils, and mineral oil, and nanoparticles frequently used include CuO, ZnO, and Alumina. In this research, laboratory-grade carbon powder were used as nanoparticle. Water was used as the fluid base in this research as the main observation focus. Carbon particles were obtain using a top-down method, whereas planetary ball mill was used to ground laboratory grade carbon powder to decrease the particle size. Milling speed and duration were set at 500 rpm and 15 hours. Field Emission Scanning Electron Microscope (FE-SEM), and Energy Dispersive X-Ray (EDX) measurement were carried out to determine the particle size, material identification, particle morphology, and surface change of samples. Nanofluid was created by mixing percentage of carbon nanoparticles with water using ultrasonic vibration for 280s. The carbon nanoparticle content in nanofluid quench mediums for this research were varied at 0.1%, 0.2%, 0.3%, 0.4, and 0.5 % volume. Furthermore, these mediums were used to quench JIS S45C or AISI 1045 carbon steel samples which austenized at 1000°C. Hardness testing and metallography observation were then conducted to further check the effect of different quench medium in steel samples. Preliminary characterizations showed that carbon particles dimension after milling was still in sub-micron stage, hundreds of nanometres to be precise. Therefore, the milling process parameters are needed to be optimized further.

Improvements in nanoscale zero-valent iron production by milling through the addition of alumina

NASA Astrophysics Data System (ADS)

Ribas, D.; Cernik, M.; Martí, V.; Benito, J. A.

2016-07-01

A new milling procedure for a cost-effective production of nanoscale zero-valent iron for environmental remediation is presented. Conventional ball milling of iron in an organic solvent as Mono Ethylene Glycol produces flattened iron particles that are unlikely to break even after very long milling times. With the aim of breaking down these iron flakes, in this new procedure, further milling is carried out by adding an amount of fine alumina powder to the previously milled solution. As the amount of added alumina increases from 9 to 54 g l-1, a progressive decrease of the presence of flakes is observed. In the latter case, the appearance of the particles formed by fragments of former flakes is rather homogeneous, with most of the final nanoparticles having an equivalent diameter well below 1 µm and with an average particle size in solution of around 400 nm. An additional increase of alumina content results in a highly viscous solution showing worse particle size distribution. Milled particles, in the case of alumina concentrations of 54 g l-1, have a fairly large specific surface area and high Fe(0) content. These new particles show a very good Cr(VI) removal efficiency compared with other commercial products available. This good reactivity is related to the absence of an oxide layer, the large amount of superficial irregularities generated by the repetitive fracture process during milling and the presence of a fine nanostructure within the iron nanoparticles.

Evaluation and development of integrated technology of rare metal concentrate production in high-level ore processing at Zashikhinsk deposit

NASA Astrophysics Data System (ADS)

Khokhulya, MS; Mukhina, TN; Ivanova, V. A.; Mitrofanova, G. V.; Fomin, A. V.; Sokolov, VD

2017-02-01

The authors discuss material constitution of columbite ore sample and recommend optimized pretreatment modes to obtain ball milling products at the maximum dissociation of ore minerals in aggregates. A concentration technology is proposed, with division of material into two flows -0.315 mm and -0.2 mm in sizes, generated in the milling and screening cycles and subjected to gravity-magnetic and magnetic-gravity treatment, respectively. It is shown that the technology ensures production of both tantalum-niobium and zircon concentrates. It has become possible to additionally recover rare metal components Nb2O5 and ZrO2 from tailings through flotation.

Studies on copper-yttria nanocomposites: high-energy ball milling versus chemical reduction method.

PubMed

Joshi, P B; Rehani, Bharati; Naik, Palak; Patel, Swati; Khanna, P K

2012-03-01

Oxide dispersion-strengthened copper-base composites are widely used for applications demanding high tensile strength, high hardness along with good electrical and thermal conductivity. Oxides of metals like aluminium, cerium, yttrium and zirconium are often used for this purpose as fine and uniformly distributed dispersoid particles in soft and ductile copper matrix. Such composites find applications as electrical contacts, resistance-welding tips, lead wires, continuous casting moulds, etc. In this investigation an attempt has been made to produce copper-yttria nanocomposites using two different morphologies of copper powder and two different processing routes namely, high-energy milling and in-situ chemical reduction. The synthesized powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) for their phase identification and morphological study. The nanocomposite powders in each case were subsequently processed to obtain bulk solids by classical powder metallurgy route of press-sinter-repress. The resultant bulk solid compacts were subjected to property evaluation. The study revealed that the properties of Cu-Y2O3 nanocomposites depend on the processing route used and in turn on the resultant powder morphology.

An investigation on the tribological properties of Co(ReO4)2/MoS2 composite as potential lubricating additive at various temperatures

NASA Astrophysics Data System (ADS)

Wang, Junhai; Lu, Bing; Zhang, Lixiu; Li, Ting; Yan, Tingting; Li, Mengxu

2018-02-01

The Co(ReO4)2 powder was fabricated via the aqueous solution method, and mixed with MoS2 powder using ball milling technique. A certain concentration of Co(ReO4)2/MoS2 composite additive was dispersed into the poly alpha olefin base oil with the assistance of surface active agents. The load-carrying property and lubricating behavior of base oil containing a certain content of Co(ReO4)2/MoS2 composite additive at various temperatures were evaluated by four-ball test and ball-on-disc sliding friction test. The physical properties and friction-reducing mechanism of synthesized composite were ascertained by a series of characterization techniques including X-ray diffraction, scanning electron microscopy-energy dispersive spectroscopy, X-ray photoelectron spectroscopy, and differential thermal analysis/thermogravimetry. The four-ball test results suggested the Co(ReO4)2/MoS2 composite additive could effectively promote the load-carrying capacity of base oil, and decrease the friction coefficient as well as wear scar diameter. Ball-on-disc sliding friction test results showed that the base oil with Co(ReO4)2/MoS2 composite additive possessed lower friction coefficients than that of base oil in the whole temperature range, particularly at high temperatures. The protective layer consisted of composite additive and native oxides from superalloy substrate formed on the worn surface to prevent the direct contact between friction pair. The Co(ReO4)2/MoS2 composite played a dominant role in friction-reducing function in the protective layer at elevated temperatures, and the reason for this was that MoS2 possessed layered structure and superior adsorption capacity, and Co(ReO4)2 had experienced thermal softening with elevated temperatures and maintained shear-susceptible hexagonal structure.

Tribo-Mechanical Properties of HVOF Deposited Fe3Al Coatings Reinforced with TiB2 Particles for Wear-Resistant Applications

PubMed Central

Amiriyan, Mahdi; Blais, Carl; Savoie, Sylvio; Schulz, Robert; Gariépy, Mario; Alamdari, Houshang

2016-01-01

This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. This study reveals the effect of TiB2 particles on the mechanical and tribological properties of Fe3Al-TiB2 composite coatings against an alumina counterpart. The feedstock was produced by milling Fe3Al and TiB2 powders in a high energy ball mill. The high-velocity oxy-fuel (HVOF) technique was used to deposit the feedstock powder on a steel substrate. The effect of TiB2 addition on mechanical properties and dry sliding wear rates of the coatings at sliding speeds ranging from 0.04 to 0.8 m·s−1 and loads of 3, 5 and 7 N was studied. Coatings made from unreinforced Fe3Al exhibited a relatively high wear rate. The Vickers hardness, elastic modulus and wear resistance of the coatings increased with increasing TiB2 content in the Fe3Al matrix. The wear mechanisms strongly depended on the sliding speed and the presence of TiB2 particles but were less dependent on the applied load. PMID:28787917

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.

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.

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.

Effect of formation temperature on properties of graphite/stannum composite for bipolar plate

NASA Astrophysics Data System (ADS)

Selamat, Mohd Zulkefli; Yusuf, Muhammad Yusri Md; Wer, Tio Kok; Sahadan, Siti Norbaya; Malingam, Sivakumar Dhar; Mohamad, Noraiham

2016-03-01

Bipolar plates are key components in Proton Exchange Membrane (PEM) fuel cells. They carry current away from the cell and withstand the clamping force of the stack assembly. Therefore, PEM fuel cell bipolar plates must have high electrical conductivity and adequate mechanical strength, in addition to being light weight and low cost in terms of both applicable materials and production methods. In this research, the raw materials used to fabricate the high performance bipolar plate are Graphite (Gr), Stannum (Sn) and Polypropylene (PP). All materials used was in powder form and Gr and Sn act as fillers and the PP acts as binder. The ratio of fillers (Gr/Sn) and binder (PP) was fixed at 80:20. For the multi-conductive filler, small amount of Sn, which is 10 up to 20wt% (from the total weight of fillers 80%) have been added into Gr/Sn/PP composite. The fillers were mixed by using the ball mill machine. The second stage of mixing process between the mixer of fillers and binder is also carried out by using ball mill machine before the compaction process by the hot press machine. The effect of formation temperatures (160°C-170°C) on the properties of Gr/Sn/PP composite had been studied in detail, especially the electrical conductivity, bulk density, hardness and microstructure analysis of Gr/Sn/PP composite. The result shows that there are significant improvement in the electrical conductivity and bulk density, which are exceeding the US-DoE target with the maximum value of 265.35 S/cm and 1.682g/cm3 respectively.

Section 2: Phase transformation studies in mechanically alloyed Fe-Nz and Fe-Zn-Si intermetallics

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

Jordan, A.; Uwakweh, O.N.C.; Maziasz, P.J.

1997-04-01

The initial stage of this study, which was completed in FY 1995, entailed an extensive analysis characterizing the structural evolution of the Fe-Zn intermetallic system. The primary interest in these Fe-Zn phases stems from the fact that they form an excellent coating for the corrosion protection of steel (i.e., automobile body panels). The Fe-Zn coating generally forms up to four intermetallic phases depending on the particular industrial application used, (i.e., galvanization, galvannealing, etc.). Since the different coating applications are non-equilibrium in nature, it becomes necessary to employ a non-equilibrium method for producing homogeneous alloys in the solid-state to reflect themore » structural changes occurring in a true coating. This was accomplished through the use of a high energy/non-equilibrium technique known as ball-milling which allowed the authors to monitor the evolution process of the alloys as they transformed from a metastable to stable equilibrium state. In FY 1996, this study was expanded to evaluate the presence of Si in the Fe-Zn system and its influence in the overall coating. The addition of silicon in steel gives rise to an increased coating. However, the mechanisms leading to the coating anomaly are still not fully understood. For this reason, mechanical alloying through ball-milling of pure elemental powders was used to study the structural changes occurring in the sandelin region (i.e., 0.12 wt % Si). Through the identification of invariant reactions (i.e., eutectic, etc.) the authors were able to explore the sandelin phenomenon and also determine the various fields or boundaries associated with the Fe-Zn-Si ternary system.« less

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

Synthesis and Characterization of Aluminum-Nanodiamond Composite Powders by High Energy Ball Milling

DTIC Science & Technology

2011-12-01

al , “ Cold - spray processing of high density nanocrystalline aluminum alloy 2009...2980, 1996. [21] L. Ajdelsztajn, et al , “ Cold spray deposition of nanocrystalline aluminum alloys ,” Metallurgical and Materials Transactions, vol...form the coating or deposit [9]. Figure 2. Diagram of a typical cold spray system [9] It has been proven that pure metals or composite powders

Controlled Synthesis and Functionalization of Vertically-Aligned Carbon Nanotubes for Multifunctional Applications

DTIC Science & Technology

2015-05-07

6 1.6 Lithium - Ion Batteries Based on Vertically-Aligned Carbon Nanotube Electrodes and Ionic...Cl, Br, or I) Prepared by Ball-Milling and Used as Anode Materials for Lithium - Ion Batteries ……………....................23 3.4 Well-Defined Two...9 1.6 Lithium - Ion Batteries Based on Vertically-Aligned Carbon Nanotube Electrodes and Ionic Liquid Electrolytes

Use of triammonium salt of aurin tricarboxylic acid as risk mitigant for aluminum hydride

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

Cortes-Concepcion, Jose A.; Anton, Donald L.

2017-08-08

A process and a resulting product by process of an aluminum hydride which is modified with by physically combining in a ball milling process an aluminum hydride with a triammonium salt of aurin tricarboxylic acid. The resulting product is an aluminum hydride which is resistant to air, ambient moisture, and liquid water while maintaining useful hydrogen storage and release kinetics.

Preparation of supported electrocatalyst comprising multiwalled carbon nanotubes

DOEpatents

Wu, Gang; Zelenay, Piotr

2013-08-27

A process for preparing a durable non-precious metal oxygen reduction electrocatalyst involves heat treatment of a ball-milled mixture of polyaniline and multiwalled carbon nanotubes in the presence of a Fe species. The catalyst is more durable than catalysts that use carbon black supports. Performance degradation was minimal or absent after 500 hours of operation at constant cell voltage of 0.40 V.

Neutralization of Aerosolized Bio-Agents by Filled Nanocomposite Materials through Thermal and Chemical Inactivation Mechanisms

DTIC Science & Technology

2016-06-01

Bio -agents by Filled Nanocomposite Materials through Thermal and Chemical Inactivation Mechanisms Distribution Statement A. Approved for public...of Cincinnati Project Title: Neutralization of Aerosolized Bio -agents by Filled Nanocomposite Materials through Thermal and Chemical Inactivation...fire ball, where they will not effectively interact with any viable bio -aerosol. 1.1.4. Conclusions Cryo-milling is necessary to achieve a

New solid state forms of antineoplastic 5-fluorouracil with anthelmintic piperazine

NASA Astrophysics Data System (ADS)

Moisescu-Goia, C.; Muresan-Pop, M.; Simon, V.

2017-12-01

The aim of the present study was to asses the formation of solid forms between the 5-fluorouracil chemotherapy drug and the anthelmintic piperazine. Two new solid forms of antineoplastic agent 5-fluorouracil with anthelmintic piperazine were obtained by liquid assisted ball milling and slurry crystallization methods. The Nsbnd H hydrogen bonding donors and C = O hydrogen bonding acceptors of 5-fluorouracil allow to form co-crystals with other drugs delivering improved properties for medical applications, as proved for other compounds of pharmaceutical interest. Both new solid forms were investigated using X-ray powder diffraction (XRD), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) spectroscopy. The XRD results show that by both methods were successfully synthesized new solid forms of 5-fluorouracil with piperazine. According to FTIR results the form prepared by lichid assisted grinding process was obtained as co-crystal and the other one, prepared by slurry method, resulted as a salt.

Facile molten salt synthesis of Li2NiTiO4 cathode material for Li-ion batteries

PubMed Central

2014-01-01

Well-crystallized Li2NiTiO4 nanoparticles are rapidly synthesized by a molten salt method using a mixture of NaCl and KCl salts. X-ray diffraction pattern and scanning electron microscopic image show that Li2NiTiO4 has a cubic rock salt structure with an average particle size of ca. 50 nm. Conductive carbon-coated Li2NiTiO4 is obtained by a facile ball milling method. As a novel 4 V positive cathode material for Li-ion batteries, the Li2NiTiO4/C delivers high discharge capacities of 115 mAh g-1 at room temperature and 138 mAh g-1 and 50°C, along with a superior cyclability. PMID:24855459

Facile Synthesis of Layer Structured GeP3/C with Stable Chemical Bonding for Enhanced Lithium-Ion Storage

NASA Astrophysics Data System (ADS)

Qi, Wen; Zhao, Haihua; Wu, Ying; Zeng, Hong; Tao, Tao; Chen, Chao; Kuang, Chunjiang; Zhou, Shaoxiong; Huang, Yunhui

2017-02-01

Recently, metal phosphides have been investigated as potential anode materials because of higher specific capacity compared with those of carbonaceous materials. However, the rapid capacity fade upon cycling leads to poor durability and short cycle life, which cannot meet the need of lithium-ion batteries with high energy density. Herein, we report a layer-structured GeP3/C nanocomposite anode material with high performance prepared by a facial and large-scale ball milling method via in-situ mechanical reaction. The P-O-C bonds are formed in the composite, leading to close contact between GeP3 and carbon. As a result, the GeP3/C anode displays excellent lithium storage performance with a high reversible capacity up to 1109 mA h g-1 after 130 cycles at a current density of 0.1 A g-1. Even at high current densities of 2 and 5 A g-1, the reversible capacities are still as high as 590 and 425 mA h g-1, respectively. This suggests that the GeP3/C composite is promising to achieve high-energy lithium-ion batteries and the mechanical milling is an efficient method to fabricate such composite electrode materials especially for large-scale application.

Enabling technologies and green processes in cyclodextrin chemistry.

PubMed

Cravotto, Giancarlo; Caporaso, Marina; Jicsinszky, Laszlo; Martina, Katia

2016-01-01

The design of efficient synthetic green strategies for the selective modification of cyclodextrins (CDs) is still a challenging task. Outstanding results have been achieved in recent years by means of so-called enabling technologies, such as microwaves, ultrasound and ball mills, that have become irreplaceable tools in the synthesis of CD derivatives. Several examples of sonochemical selective modification of native α-, β- and γ-CDs have been reported including heterogeneous phase Pd- and Cu-catalysed hydrogenations and couplings. Microwave irradiation has emerged as the technique of choice for the production of highly substituted CD derivatives, CD grafted materials and polymers. Mechanochemical methods have successfully furnished greener, solvent-free syntheses and efficient complexation, while flow microreactors may well improve the repeatability and optimization of critical synthetic protocols.

Novel Preparation of Calcium Borate/Graphene Oxide Nanocomposites and Their Tribological Properties in Oil

NASA Astrophysics Data System (ADS)

Li, Wei; Cheng, Zhi-Lin; Liu, Zan

2017-01-01

The calcium borate/graphene oxide (CB/GO) nanocomposites have been successfully prepared by a liquid phase-based ultrasonic-assisted stripping method, which were subsequently explored as lubricant additive. The structure and morphology of the as-prepared nanocomposites were characterized by FT-IR, XRD, Raman, TEM, EDS and TGA, revealing that CB nanoparticles were uniformly loaded on GO surfaces. The nanocomposites were highly dispersed into the base oil by sand milling. The tribological properties of CB/GO nanocomposites as lubricating oil additive were investigated using a four-ball machine, and the wear scar surfaces were observed by the 3D Laser Scanning Microscope. The results indicated that CB/GO nanocomposites were of excellent antifriction, antiwear ability and load-carrying capacity.

Magnetic enhancement and coding in mechanosynthesized Ni{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} nanoparticles

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

Majumder, S.; Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata-700064; Dey, S.

2015-06-24

The nanosized Ni{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} (∼ 15 nm) has been synthesized by high energy ball milling of the bulk powder sample. The sample has been characterized by powder x-ray diffraction, field emission and transmission electron microscopic and dc magnetic measurement techniques. The dc magnetic measurement on the sample indicates that the sample exhibit enhancement of magnetization compared to its counterparts synthesized by chemical methods. Moreover, the system stores the memory of either decrease or increase of magnetic field enabling a magnetic coding of “0” and “1” which can be profitably used in magnetic storage and sensing devices.

Rapid Aluminum Nanoparticle Production by Milling in NH₃ and CH₃NH₂ Atmospheres: An Experimental and Theoretical Study.

PubMed

McMahon, Brandon W; Yu, Jiang; Boatz, Jerry A; Anderson, Scott L

2015-07-29

Ball milling of aluminum in gaseous atmospheres of ammonia and monomethylamine (MMA) was found to produce particles in the 100 nm size range with high efficiency. A combination of mass spectrometry, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis with mass spectrometric product analysis (TGA-MS), scanning electron microscopy (SEM), infrared spectroscopy, and dynamic light scattering (DLS) was used to study the particles and the chemical interactions responsible for particle production. To help understand the nature of the surface chemistry, high level quantum chemical calculations were performed to predict the structures and energetics for binding and reactions of NH3 and MMA on aluminum surfaces. Both NH3 and MMA react with aluminum under milling conditions, producing H2 and other gaseous products, and leaving the surfaces functionalized. The surface functionalization enhances size reduction by reducing the surface free energy and the tendency toward mechanochemical welding. For both NH3 and MMA, the particle cores are metallic aluminum, but the surface chemical properties are quite different. The ammonia-milled particles are capped by an AlNxOyHz layer ∼10 nm thick, which passivates the particles. The MMA-milled particles are capped with a thinner passivating layer, such that they are pyrophoric in air and react with N2 at elevated temperatures.

Development of a Novel Ni-Fe-Cr-B-Si Interlayer Material for Transient Liquid Phase Bonding of Inconel 718

NASA Astrophysics Data System (ADS)

Tarai, U. K.; Robi, P. S.; Pal, Sukhomay

2018-04-01

A Ni-Cr-Fe-Si-B based interlayer material was developed by mechanical alloying (MA) process in a high-energy planetary ball mill. Equiaxed alloy powders of size 12 µm was obtained after milling for 50 hours. X-ray diffraction analysis of the milled powder revealed that milling of elemental powders initially resulted in microcrystalline alloy powder having face centered cubic structure, which on subsequent milling resulted in nano-crystallice alloy powder with a crystallite size of 3.2 nm. XRD analysis also reveals formation of metastable eutectic alloys resulting in lowering of the melting point of the interlayer material to 1025 °C. IN 718 superalloy samples were joined at 1050°C using the developed interlayer. A homogeneous joint was formed by the newly developed interlayer material. Three different zones were observed at the bond (i) isothermally solidified zone, (ii) diffusion affected zone and (iii) unaffected base metal. In the diffusion-affected zone, boron was present at the grain boundaries of Ni γ matrix in bulky metal borides form. The diffusion of boron from interlayer material into the base material was mechanism of isothermal solidification and bond formation in transient liquid phase bonding of IN 718.

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

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.

Simulation-Assisted Evaluation of Grinding Circuit Flowsheet Design Alternatives: Aghdarreh Gold Ore Processing Plant / Ocena Alternatywnych Schematów Technologicznych Procesu Rozdrabniania W Zakładach Przeróbki Rud Złota W Aghdarreh, Z Wykorzystaniem Metod Symulacji

NASA Astrophysics Data System (ADS)

Farzanegan, A.; Ghalaei, A. Ebtedaei

2015-03-01

The run of mine ore from Aghdarreh gold mine must be comminuted to achieve the desired degree of liberation of gold particles. Currently, comminution circuits include a single-stage crushing using a jaw crusher and a single-stage grinding using a Semi-Autogenous Grinding (SAG) mill in closed circuit with a hydrocyclone package. The gold extraction is done by leaching process using cyanidation method through a series of stirred tanks. In this research, an optimization study of Aghdarreh plant grinding circuit performance was done to lower the product particle size (P80) from 70 μm to approximately 40 μm by maintaining current throughput using modeling and simulation approach. After two sampling campaigns from grinding circuit, particle size distribution data were balanced using NorBal software. The first and second data sets obtained from the two sampling campaigns were used to calibrate necessary models and validate them prior to performing simulation trials using MODSIM software. Computer simulations were performed to assess performance of two proposed new circuit flowsheets. The first proposed flowsheet consists of existing SAG mill circuit and a new proposed ball mill in closed circuit with a new second hydrocyclone package. The second proposed flowsheet consists of existing SAG mill circuit followed by a new proposed ball mill in closed circuit with the existing hydrocyclone package. In all simulations, SAGT, CYCL and MILL models were selected to simulate SAG mill, Hydrocyclone packages and ball mill units. SAGT and MILL models both are based on population balance model of grinding process. CYCL model is based on Plitt's empirical model of classification process in hydrocyclone units. It was shown that P80 can be reduced to about 40 μm and 42 μm for the first and second proposed circuits, respectively. Based on capital and operational costs, it can be concluded that the second proposed circuit is a more suitable option for plant grinding flowsheet modification. Surowy urobek z kopalni rud złota Aghdarreh musi najpierw zostać poddany rozdrobnieniu, aby zapewnić efektywniejsze uwalnianie cząsteczek złota. W chwili obecnej obiegi rozdrabniania obejmują kruszenie jednostopniowe z wykorzystaniem kruszarek szczękowych oraz kruszenie jednostopniowe z użyciem kruszarek półautomatycznych w obiegu zamkniętym z hydrocyklonem. Odzysk złota odbywa się przy zastosowaniu procesu ługowania, z zastosowaniem metody cyjankowej w szeregu mieszalników. W pracy tej przeprowadzono optymalizację procesu rozdrabniania rud w zakładach przeróbczych Aghdarreh prowadzonego w celu zmniejszenia rozmiarów uzyskiwanych cząsteczek złota (Ps0) z 70 μm do ok. 40 μm poprzez zapewnienie ciągłości procesu, z wykorzystaniem metod modelowania i symulacji. Na podstawie dwóch zestawów próbek z ciągu technologicznego rozdrabniania, rozkłady wielkości cząstek zostały statystycznie zrównoważone z wykorzystaniem oprogramowania NorBal. Pierwszy i drugi zbiór danych otrzymanych na podstawie dwóch zestawów próbek wykorzystany został do kalibracji i walidacji modeli, przed przystąpieniem do właściwych badań symulacyjnych z użyciem oprogramowania MODSIM. Symulacje komputerowe przeprowadzono w celu oceny wydajności dwóch proponowanych ciągów technologicznych. Pierwszy ciąg obejmuje istniejące kruszarki półautomatyczne i nowo proponowaną kruszarkę kulową pracującą w obiegu zamkniętym z hydrocyklonem. Drugi rozważany ciąg stanowi istniejąca kruszarka półautomatyczna, następnie proponowana kruszarka kulowa pracująca w obiegu zamkniętym z istniejącym hydrocyklonem. We wszystkich symulacjach bazowano na modelach SAGT, CYCL i MILL do symulacji pracy kruszarek półautomatycznych, pakietu hydrocyklonu oraz pojedynczych kruszarek. Modele SAGT i MILL oparte są na modelu zrównoważonej populacji w procesie rozdrabniania. Model CYCL opiera się na empirycznym modelu klasyfikacji Plitta zastosowanym do hydrocyklonów. Wykazano, że rozmiar cząstek zmniejszony został odpowiednio do 40 μm i 42 μm dla pierwszego i drugiego analizowanego obiegu. Uwzględniając nakłady kapitałowe oraz koszty operacyjne, wyciągnąć można więc wniosek, ze drugi proponowany układ jest korzystniejszą opcją modyfikacji istniejącego ciągu technologicznego rozdrabniania.

Use of triphenyl phosphate as risk mitigant for metal amide hydrogen storage materials

DOEpatents

Cortes-Concepcion, Jose A.; Anton, Donald L.

2016-04-26

A process in a resulting product of the process in which a hydrogen storage metal amide is modified by a ball milling process using an additive of TPP. The resulting product provides for a hydrogen storage metal amide having a coating that renders the hydrogen storage metal amide resistant to air, ambient moisture, and liquid water while improving useful hydrogen storage and release kinetics.

Solution-state 2D NMR of ball-milled plant cell wall gels in DMSO-d6/pyridine-d5†

PubMed Central

Ralph, John

2014-01-01

NMR fingerprinting of the components of finely divided plant cell walls swelled in DMSO has been recently described. Cell wall gels, produced directly in the NMR tube with perdeutero-dimethylsulfoxide, allowed the acquisition of well resolved/dispersed 2D 13C–1H correlated solution-state NMR spectra of the entire array of wall polymers, without the need for component fractionation. That is, without actual solubilization, and without apparent structural modification beyond that inflicted by the ball milling and ultrasonication steps, satisfactorily interpretable spectra can be acquired that reveal compositional and structural details regarding the polysaccharide and lignin components in the wall. Here, the profiling method has been improved by using a mixture of perdeuterated DMSO and pyridine (4:1, v/v). Adding pyridine provided not only easier sample handling because of the better mobility compared to the DMSO-d6-only system but also considerably elevated intensities and improved resolution of the NMR spectra due to the enhanced swelling of the cell walls. This modification therefore provides a more rapid method for comparative structural evaluation of plant cell walls than is currently available. We examined loblolly pine (Pinus taeda, a gymnosperm), aspen (Populus tremuloides, an angiosperm), kenaf (Hibiscus cannabinus, an herbaceous plant), and corn (Zea mays L., a grass, i.e., from the Poaceae family). In principle, lignin composition (notably, the syringyl : guaiacyl : p-hydroxyphenyl ratio) can be quantified without the need for lignin isolation. Correlations for p-coumarate units in the corn sample are readily seen, and a variety of the ferulate correlations are also well resolved; ferulates are important components responsible for cell wall cross-linking in grasses. Polysaccharide anomeric correlations were tentatively assigned for each plant sample based on standard samples and various literature data. With the new potential for chemometric analysis using the 2D NMR fingerprint, this gel-state method may provide the basis for an attractive approach to providing a secondary screen for selecting biomass lines and for optimizing biomass processing and conversion efficiencies. PMID:20090974

Oily nanosuspension for long-acting intramuscular delivery of curcumin didecanoate prodrug: preparation, characterization and in vivo evaluation.

PubMed

Wei, Xiao-Lan; Han, Ying-Rui; Quan, Li-Hui; Liu, Chun-Yu; Liao, Yong-Hong

2013-05-13

The objective of this study was to prepare the nanocrystals of curcumin didecanoate (CurDD) by wet ball milling and to investigate the comparative pharmacokinetics of oily nano- and micro-suspensions after intramuscular (i.m.) administration to rats. Upon optimizing the wet ball milling parameters, CurDD nanocrystals were produced with median particle size of ~500 nm and the freeze-dried nanocrystals were readily dispersed in peanut oil to form stable nanosuspensions. Although the nanosuspension appeared to exhibit slower clearance from the injection site after i.m. injection, compared to microsuspension (~5 μm), a significantly higher maximum plasma curcumin concentration (69.0 ng/ml) was observed for the former than that for the latter (18.5 ng/ml). In addition, the nanosuspension provided significant higher plasma curcumin concentrations and brain CurDD contents for at least 15 days than the microsuspension, except for the initial times. A single i.m. injection of nanosuspension appeared to achieve reversal effect on reserpine-induced hypothermia for at least 13 days. This study demonstrates that CurDD nanosuspension may act as a long-acting i.m. injectable for sustained delivery of curcumin, potentially applicable to elicit a long-lasting antidepressant effect. Copyright © 2013 Elsevier B.V. All rights reserved.

Release of Polyphenols Is the Major Factor Influencing the Bioconversion of Rice Straw to Lactic Acid.

PubMed

Chen, Xingxuan; Xue, Yiyun; Hu, Jiajun; Tsang, Yiu Fai; Gao, Min-Tian

2017-11-01

In this study, we found that p-coumaric acid (p-CA), ferulic acid (FA), and condensed tannins were released from rice straw during saccharification. The presence of polyphenols prolonged the lag phase and lowered the productivity of lactic acid. p-CA was identified as a key inhibitor. Tannins had a lower inhibitory effect than p-CA; FA had little inhibitory effect. Acid, alkaline, and ball milling pretreatments elicited different levels of polyphenol release from rice straw. Due to the different levels of polyphenol release in the pretreatment step, the enzymatic hydrolysates contained different concentrations of polyphenols. Compared with fermentation with a synthetic medium, fermentation with the hydrolysates of ball-milled rice straw provided much lower productivity and yield of lactic acid due to the presence of polyphenols. Removal of these compounds played an important role in lactic acid fermentation. When rice straw was alkaline pretreated, the hydrolysates contained few phenolic compounds, resulting in high productivity and yield of lactic acid (1.8 g/L/h and 26.7 g/100 g straw), which were comparable to those in a synthetic medium. This indicates that there is a correlation between removal of phenolic compounds and efficiency in lactic acid fermentation.

Structure and magnetic properties of L10-MnGa nanoparticles prepared using direct reactions between Mn nanoparticles and Ga

NASA Astrophysics Data System (ADS)

Si, P. Z.; Qian, H. D.; Park, J.; Ge, H. L.; Shinde, K. P.; Chung, K. C.; Choi, C. J.

2018-05-01

The tetragonal L10-Mn1+xGa (x<0.8) nanoparticles and bcc-Mn23Ga77 nanoparticles with large coercivity were prepared using direct reactions between Mn nanoparticles and Ga at elevated temperatures. The Mn23Ga77 phase was formed at ˜573 K while the L10-structured Mn1+xGa was formed at ˜850 K. After ball-milling, the L10-Mn1+xGa nanoparticles transformed into nano-flakes with enhanced coercivity. The size of the as-prepared Mn23Ga77 nanoparticles is comparable to that of the precursor Mn nanoparticles. An aggregation of the nanoparticles and thus a larger particle size were observed in the L10-Mn1+xGa nanoparticles obtained at 850 K. The size of the L10-Mn1+xGa nano-flakes is reduced to about 200-400 nm with a thickness of ˜20 nm. The coercivity of the Mn23Ga77 nanoparticles and the L10-Mn1+xGa nanoparticles at 300 K reached up to 0.2 T and 0.43 T, respectively. The coercivity of L10-Mn1+xGa ball-milled nano-flakes is 0.59 T at 300 K.

Electrical and dielectric properties of Na1/2La1/2Cu3Ti4O12 ceramics prepared by high energy ball-milling and conventional sintering

NASA Astrophysics Data System (ADS)

Mahfoz Kotb, H.; Ahmad, Mohamad M.

2016-12-01

We report on the measurements of the electrical and dielectric properties of Na1/2La1/2Cu3Ti4O12 (NLCTO) ceramics prepared by high energy ball-milling and conventional sintering without any calcination steps. The x-ray powder diffraction analysis shows that pure perovskite-like CCTO phase is obtained after sintering at 1025 °C-1075 °C. Higher sintering temperatures result in multi-phase ceramics due to thermal decomposition. Scanning electron microscope observations reveal that the grain size is in a range of ˜3 μm-5μm for these ceramics. Impedance spectroscopy measurements performed in a wide frequency range (1 Hz-10 MHz) and at various temperatures (120 K-470 K) are used to study the dielectric and electrical properties of NLCTO ceramics. A good compromise between high ɛ‧ (5.7 × 103 and 4.1 × 103 at 1.1 kHz and 96 kHz, respectively) and low tan δ (0.161 and 0.126 at 1.1 kHz and 96 kHz, respectively) is obtained for the ceramic sintered at 1050 °C. The observed high dielectric constant behavior is explained in terms of the internal barrier layer capacitance effect.

The grinding behavior of ground copper powder for Cu/CNT nanocomposite fabrication by using the dry grinding process with a high-speed planetary ball mill

NASA Astrophysics Data System (ADS)

Choi, Heekyu; Bor, Amgalan; Sakuragi, Shiori; Lee, Jehyun; Lim, Hyung-Tae

2016-01-01

The behavior of ground copper powder for copper-carbon nanotube (copper-CNT) nanocomposite fabrication during high-speed planetary ball milling was investigated because the study of the behavior characteristics of copper powder has recently gained scientific interest. Also, studies of Cu/CNT composites have widely been done due to their useful applications to enhanced, advanced nano materials and components, which would significantly improve the properties of new mechatronics-integrated materials and components. This study varied experimental conditions such as the rotation speed and the grinding time with and without CNTs, and the particle size distribution, median diameter, crystal structure and size, and particle morphology were monitored for a given grinding time. We observed that pure copper powders agglomerated and that the morphology changed with changing rotation speed. The particle agglomerations were observed with maximum experiment conditions (700 rpm, 60 min) in this study of the grinding process for mechanical alloys in the case of pure copper powders because the grinding behavior of Cu/CNT agglomerations was affected by the addition of CNTs. Indeed, the powder morphology and the crystal size of the composite powder could be changed by increasing the grinding time and the rotation speed.

Sintering temperature effect of divalent europium ion doped tetra-calcium phosphate phosphors for latent fingerprint detection

NASA Astrophysics Data System (ADS)

Hong, Woo Tae; Park, Jin Young; Je, Jae-Yong; Yang, Hyun Kyoung

2018-07-01

Ca4(PO4)2O:Eu2+ (CPO:Eu2+) phosphors were successfully synthesized by high-energy ball milling. In order to study the effect of sintering temperature, the phosphors were synthesized at various sintering temperatures. The crystal structure of CPO:Eu2+ was determined to be monoclinic P21. Owing to the f-d transitions of the Eu2+ ions in the CPO:Eu2+ phosphors, the PL spectra of the phosphors showed an intense red emission centered at 635 nm with 418 nm excitation. Using high-energy ball milling, a more intense emission (compared to that reported from other research) can be visually observed with human eyes in the form of orange-red light, which is helpful in latent fingerprint detection. In addition, high-temperature sintering results in an increase of the PL intensity owing to the larger particle size and lower levels of impurities in the CPO:Eu2+ phosphors. The latent fingerprint image obtained by using CPO:Eu2+ phosphors reveals a high contrast for various substrate materials, because the phosphors exhibit strong red emission and adhere to the residue of the fingerprint after flowing. On the basis of these results, red-emitting CPO:Eu2+ phosphors can be used for the detection of latent fingerprints in solving criminal cases.

Lithium silicide nanocrystals: synthesis, chemical stability, thermal stability, and carbon encapsulation.

PubMed

Cloud, Jacqueline E; Wang, Yonglong; Li, Xuemin; Yoder, Tara S; Yang, Yuan; Yang, Yongan

2014-10-20

Lithium silicide (LixSi) is the lithiated form of silicon, one of the most promising anode materials for the next generation of lithium-ion batteries (LIBs). In contrast to silicon, LixSi has not been well studied. Herein we report a facile high-energy ball-milling-based synthesis of four phase-pure LixSi (x = 4.4, 3.75, 3.25, and 2.33), using hexane as the lubricant. Surprisingly, the obtained Li3.75Si phase shows significant downward shifts in all X-ray diffraction peak positions, compared with the standard. Our interpretation is that the high-energy ball-mill-synthesized Li3.75Si presents smaller internal pressures and larger lattice constants. The chemical-stability study reveals that only surface reactions occur after Li4.4Si and Li3.75Si are immersed in several battery-assembly-related chemicals. The thermal-stability study shows that Li4.4Si is stable up to 350 °C and Li3.75Si is stable up to 200 °C. This remarkable thermal stability of Li3.75Si is in stark contrast to the long-observed metastability for electrochemically synthesized Li3.75Si. The carbon encapsulation of Li4.4Si has also been studied for its potential applications in LIBs.

Mechanochemical destruction of DDTs with Fe-Zn bimetal in a high-energy planetary ball mill.

PubMed

Sui, Hong; Rong, Yuzhou; Song, Jing; Zhang, Dongge; Li, Haibo; Wu, Peng; Shen, Yangyang; Huang, Yujuan

2018-01-15

Mechanochemical destruction has been proposed as a promising, non-combustion technology for the disposal of toxic, halogenated, organic pollutants. In the study presented, additives including Fe, Zn, Fe-Zn bimetal, CaO and Fe 2 O 3 were tested for their effectiveness to remove DDTs by MC. The results showed that Fe-Zn bimetal was the most efficient additive, with 98% of DDTs removed after 4h. The Fe-Zn mass ratio was optimized to avoid possible spontaneous combustion of the ground sample during subsample collection. Inorganic water-soluble chloride in the ground sample increased by 91% after 4h of grinding, which indicated dechlorination during destruction of DDTs. In addition, relationships were established between the rate constant and the rotation speed or the charge ratio. Discrete Element Method (DEM) modeling was used to simulate the motion of the grinding ball and calculate both total impact energy and normal impact energy. The latter expressed a stronger, linear correlation with the rate constant. Therefore, normal impact energy is proposed to be the main driving force in the MC destruction of DDTs. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of plutonium-bearing ceramics via mechanically activated precursor

NASA Astrophysics Data System (ADS)

Chizhevskaya, S. V.; Stefanovsky, S. V.

2000-07-01

The problem of excess weapons plutonium disposition is suggested to be solved by means of its incorporation in stable ceramics with high chemical durability and radiation resistivity. The most promising host phases for plutonium as well as uranium and neutron poisons (gadolinium, hafnium) are zirconolite, pyrochlore, zircon, zirconia [1,2], and murataite [3]. Their production requires high temperatures and a fine-grained homogeneous precursor to reach final waste form with high quality and low leachability. Currently various routes to homogeneous products preparation such as sol-gel technology, wet-milling, and grinding in a ball or planetary mill are used. The best result demonstrates sol-gel technology but this route is very complicated. An alternative technology for preparation of ceramic precursors is the treatment of the oxide batch with high mechanical energy [4]. Such a treatment produces combination of mechanical (fine milling with formation of various defects, homogenization) and chemical (split bonds with formation of active centers—free radicals, ion-radicals, etc.) effects resulting in higher reactivity of the activated batch.

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.

Date palm waste-derived biochar composites with silica and zeolite: synthesis, characterization and implication for carbon stability and recalcitrant potential.

PubMed

Ahmad, Munir; Ahmad, Mahtab; Usman, Adel R A; Al-Faraj, Abdullah S; Abduljabbar, Adel; Ok, Yong Sik; Al-Wabel, Mohammad I

2017-03-23

Engineered organo-mineral composites were synthesized from date palm waste biochar and silica or zeolite via mechanochemical treatments. Date palm tree rachis (leaves) waste biomass was pre-treated with silica or zeolite minerals via ball milling and sonication prior to pyrolysis at 600 °C. The resultant organo-mineral composites and pristine materials were characterized using X-ray diffraction, thermogravimetric-differential thermal (TG-DTA), Fourier transform infrared, scanning electron microscope analyses and surface area and porosity analyzer to investigate the variations in physiochemical and structural characteristics. Compared to the resultant composites derived from non-milled date palm biomass, ball milling increased surface area, while decreased crystallinity index and effective particle size of the biochar composites. Silica composited biochars were located near origin in the van Krevelen diagram indicating lowest H/C and O/C molar ratios, thus suggesting higher aromaticity and lower polarity compared to other biochars. TGA thermograms indicated highest thermal stability of silica composited biochars. Ash and moisture corrected TGA thermograms were used to calculate recalcitrance index (R 50 ) of the materials, which speculated high degradability of biomass (R 50  < 0.4), minimal degradability of biochars and zeolite composited biochars (0.5 < R 50  < 0.7) and high recalcitrant nature of silica composited biochars (R 50  > 0.7). Silica composited biochars exhibited highest carbon sequestration potential (64.17-95.59%) compared to other biochars. Highest recalcitrance and carbon sequestration potential of silica composited biochars may be attributed to changes in structural arrangements in the silica-biochar complex. Encapsulations of biochar particles with amorphous silica via Si-C bonding may have prevented thermal degradation, subsequently increasing recalcitrance potential of silica composited biochars.

Preparation, consolidation, and crystallization of bulk metallic glasses

NASA Astrophysics Data System (ADS)

Holland, Troy

Bulk metallic glasses (BMGs) have been widely researched over the last decade. Research has primarily focused on BMGs of differing compositions and conditions within 3 main subject areas: preparation, consolidation, and crystallization. This work endeavors to show the interrelationships among each area across several types of BMG. Two compositions of zirconium(Zr)-type BMGs were prepared by mechanical attrition using a high-energy ball mill. The thermal and x-ray diffraction show that by milling elemental powders it is possible to obtain metallic powders with a glassy nature. These powders were then consolidated using a novel, high current density hot press. Hot pressing by using a spark plasma sintering (SPS) device has shown itself to be very useful in consolidating hard to produce intermetallics and ceramics. By utilizing high current densities and extremely rapid heating rates, the consolidation of the Zr-type ball milled powders and a gas atomized iron(Fe)-type powder was achieved. Utilizing the Kissinger relationship between reaction temperatures and their heating rates allowed for higher peak consolidation temperatures without fully- or partially-devitrifying the powders. The current densities applied aid in the diffusion and thermodynamics of the devitrification reaction. This affect has had little to no previous research so it was necessary to determine the specific effects of applied currents upon the devitrification of BMGs. To determine the role of applied currents on crystallization, or devitrification, of BMGs required the application of differing currents at fixed annealing temperatures. Once this was achieved it was possible with small-angle neutron scattering (SANS), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM) to show that both the kinetics and thermodynamics of the devitrification reaction were affected.

Mixed Metal Oxides of the Type CoxZn1-xFe2O4 as Photocatalysts for Malachite Green Degradation Under UV Light Irradiation.

PubMed

Tzvetkov, Martin; Milanova, Maria; Cherkezova-Zheleva, Zara; Spassova, Ivanka; Valcheva, Evgenia; Zaharieva, Joana; Ivan, Mitov

2017-06-01

A combination of thermal and mechanical (high energy ball milling) treatment was applied in an attempt to obtain polycrystalline mixed metal binary and ternary oxides of the type CoxZn1-xFe2O4 (x = 0; 0.25; 0.5; 0.75; 1). The synthetic procedure used successfully produced single-phased, homogeneous ZnFe2O4, CoFe2O4, and Co0.75Zn0.25Fe2O4, as well as mixed oxides, whose composition depended both on the duration of the high energy ball milling and the ratio Zn(II)/Co(II). The formation of spinel-like structures was proved by XRD, Mössbauer spectroscopy and Raman spectroscopy. For the characterization of the samples low-temperature N2 adsorption, UV/Vis spectroscopy and transmission electron microscopy were applied. The energy band gap of the samples was calculated, suggesting they are promising photocatalysts. The decomposition of the Malachite Green in model water solutions under UV-light irradiation was successfully achieved in the presence of the samples as photocatalysts. The highest rate constant was obtained for the sample synthesized at longer milling time in combination with higher Zn(II)/Co(II) ratio. The photocatalytic activity of the ternary mixed oxides was compared with the pure hematite, α-Fe2O3, and the binary ZnFe2O4 and CoFe2O4 ferrites with spinel structure that were treated in the same way. A synergetic effect of α-Fe2O3 and the spinel-like structure on the photocatalytic properties of ternary mixed metal oxides was detected.

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).

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.

High temperature ferromagnetism in Ni doped ZnO nanoparticles: Milling time dependence

NASA Astrophysics Data System (ADS)

Pal, Bappaditya; Giri, P. K.; Sarkar, D.

2014-04-01

We report on the room temperature ferromagnetism (RT FM) in the Zn1-xNixO (x = 0, 0.03, and 0.05) nanoparticles (NPs) synthesized by a ball milling technique. X-ray diffraction analysis confirms the single crystalline ZnO wurtzite structure with presence of small intensity secondary phase related peak which disappear with increasing milling time for Ni doped samples. HRTEM lattice images show that the doped NPs are single crystalline with a dspacing of 2.44 Å. Energy-dispersive X-ray spectroscopy analysis confirms the presence of Ni ions in the ZnO matrix. Magnetic measurement (RT) exhibits the hysteresis loop with saturation magnetization (Ms) of 1.6-2.56 (emu/g) and coercive field (Hc) of 296-322 Oe. M-T measurement shows a Curie temperature of the order of 325°C for 3% Ni doped sample. Micro -Raman studies show doping/disorder induced additional modes at ˜510, 547, 572 cm-1 in addition to 437 cm-1 peak of pure ZnO. UV-Vis absorption spectra illustrate band gap shift due to doping. Alteration of Ms value with the variation of doping concentration and milling time has been studied and discussed.

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.

Systems and methods for the synthesis of high thermoelectric performance doped-SnTe materials

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

Ren, Zhifeng; Zhang, Qian; Chen, Gang

A thermoelectric composition comprising tin (Sn), tellurium (Te) and at least one dopant that comprises a peak dimensionless figure of merit (ZT) of 1.1 and a Seebeck coefficient of at least 50 .mu.V/K and a method of manufacturing the thermoelectric composition. A plurality of components are disposed in a ball-milling vessel, wherein the plurality of components comprise tin (Sn), tellurium (Te), and at least one dopant such as indium (In). The components are subsequently mechanically and thermally processed, for example, by hot-pressing. In response to the mechanical-thermally processing, a thermoelectric composition is formed, wherein the thermoelectric composition comprises a dimensionlessmore » figure of merit (ZT) of the thermoelectric composition is at least 0.8, and wherein a Seebeck coefficient of the thermoelectric composition is at least 50 .mu.V/K at any temperature.« less

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.

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") kinetics improve with increased number of fold and roll (FR) operations. With increasing FR operations the distribution of the Ti phase is progressively refined, and the shape of the absorption curve no longer remains sigmoidal. Up to a point, increasing the loading amount of the second phase also accelerates the kinetics. Microscopy analysis performed on 1--2 wt.% hydrogen absorbed composites demonstrates that MgH 2 formed exclusively on various heterogeneous nucleation sites. During activation, MgH2 nucleation occurred at the Mg-hard phase interfaces. On the subsequent absorption cycles, heterogeneous nucleation primarily occurred in the vicinity of "internal" free surfaces such as cracks.

Fabrication and Optimization of Carbon Nanomaterial-Based Lithium-Ion Battery Anodes

DTIC Science & Technology

2012-03-01

preparation setup under the fume hood with NMP solvent, glass pipette with dispenser, and the ball milled powder mixture containing LiFePO4 , acetylene...minutes. ............................................................................. 18 Figure 12. (a) LiFePO4 slurry applied on foil current collector...and (b) LiFePO4 slurry casted with applicator and (c) LiFePO4 casted (From [15])....... 18 Figure 13. MTI disc cutter used to cut individual

Preparation of nano fluids by mechanical method

NASA Astrophysics Data System (ADS)

Boopathy, J.; Pari, R.; Kavitha, M.; Angelo, P. C.

2012-07-01

Nanofluids are conventional heat transfer fluids that contain nano particles of metals, oxides, carbides, nitrides, or nanotubes. Nanofluids exhibit enhanced thermal conductivity and heat transfer coefficients compared to the base fluids. This paper presents the procedure for preparing nanofluids consisting of Copper and Aluminium nano powders in base fluids. Copper and Aluminium nano powders were produced by planetary ball wet milling at 300rpm for 50hrs. Toluene was added to ensure wet milling. These powders were characterized in XRD and SEM for their purity, particle size and shape. The XRD results confirmed the final particle sizes of Copper and Aluminium in the nano range. Then the 0.01 gm of nano metal powders was added in 150 ml of double distilled water and magnetic stirring was done at 1500 rpm for 15 minutes. Sodium lauryl sulphate (0.05%) was added in water as surfactant to ensure the stability of the dispersion. Ultrasonication in the 3000 watts bath was done for 10 minutes to enhance the uniform dispersion of metal powders in water. The pH, dynamic viscosity, ionic conductivity and the stability of the fluids were determined for further usage of synthesized nanofluids as coolant during grinding operation.

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.