Effect of ball milling time on the microstructure and compressive properties of the Fe–Mn–Al porous steel

In the present work,Fe–Mn–Al–C powder mixtures were manufactured by elemental powders with different ball milling time,and the porous high-Mn and high-Al steel was fabricated by powder sintering.The results indicated that the powder size significantly decreased,and the morphology of the Fe powder tended to be increasingly flat as the milling time increased.However,the prolonged milling duration had limited impact on the phase transition of the powder mixture.The main phases of all the samples sintered at 640℃ were α-Fe,α-Mn and Al,and a small amount of Fe2Al5 and Al8Mn5.When the sintering temperature increased to 1200℃,the phase composition was mainly comprised of γ-Fe and α-Fe.The weight loss fraction of the sintered sample decreased with milling time,i.e.,8.3wt% after 20 h milling compared to15.3wt% for 10 h.The Mn depletion region(MDR) for the 10,15,and 20 h milled samples was about 780,600,and 370 μm,respectively.The total porosity of samples sintered at 640℃ decreased from ~46.6vol% for the 10 h milled powder to ~44.2vol% for 20 h milled powder.After sintering at 1200℃,the total porosity of sintered samples prepared by 10 and 20 h milled powder was ~58.3vol% and ~51.3vol%,respectively.The compressive strength and ductility of the 1200℃ sintered porous steel increased as the milling time increased.

Low-Temperature Synthesis of Nano-AlN Based on Solid Nitrogen Source by Plasma-Assisted Ball Milling

Plasma-assisted ball milling was carried out on the Al+C3H6N6 system and Al+C_(4)H_(4)N_(4) system,respectively.The phase structure,functional groups and synthesis mechanism were analyzed by XRD and FT-IR,and the differences in the synthesis process of nano-AlN with different solid nitrogen sources were discussed.The results show that C3H6N6 has a stable triazine ring structure,and its chemical bond is firm and difficult to break,so AlN cannot be synthesized directly by solid-solid reaction at room temperature.However,there are a large number of nitrile groups(-CN)and amino groups(-NH_(2))in C_(4)H_(4)N_(4) molecules.Under the combined action of plasma bombardment and mechanical energy activation,C_(4)H_(4)N_(4) molecules undergo polycondensation and deamination,so that the ball milling tank is filled with a large number of active nitrogen-containing groups such as N=,≡N,etc.These groups and ball milling activated Al can synthesize nano-AlN at room temperature,with a conversion rate of 92%.SEM,DSC/TG analysis showed that the powder obtained by ball milling was formed by soft agglomeration of many fine primary particles about 50–80 nm.The surface morphology of the powder was loose and porous,and it had strong activity.After annealing at 800℃,the conversion rate of the Al+C_(4)H_(4)N_(4) system reached 99%.

Mechanochemical decomposition of pentachlorophenol by ball milling

The mechanochemical dechlorination of pentachlorophenol （PCP） was studied using CaO and SiO2 powder as additives. The effects of the milling time and additives on the dechlorination rate were investigated. The resulting product was characterized by X-ray diffraction （XRD）, Fourier transform infrared spectra （FT-IR）, thermogravimetric analysis （TG） and ion chromatography （IC）. It is found that grinding operation could dechlorinate PCP, with the formation of inorganic chloride and amorphous carbon. The addition of quartz to the grinding mixture facilitated dechlorination. On the basis of the experimental results, the decomposition mechanism was proposed. Decomposition predominantly proceeds through rupture of C-Cl bond in PCP molecule, followed by the formation of inorganic chlorides.

Microstructure and electrical properties of Y_2O_3-doped ZnO-based varistor ceramics prepared by high-energy ball milling

Y2O3-doped ZnO-based varistor ceramics were prepared using high-energy ball milling （HEBM） and low-temperature sin- tering technique, with voltage-gradient of 1934-2197 V/mm, non-linear coefficients of 20.8-21.8, leakage currents of 0.59-1.04 μA, and densities of 5.46-5.57 g/cm3. With increasing Y2O3 content, the voltage-gradient increases because of the decrease of ZnO grain size; the non-linear coefficient and the leakage current improve but the density decreases because of more porosity; the donor con- centration and density of interface states decrease, whereas the barrier height and width increase because of the acceptor effect of Y2O3 in varistor ceramics.

Microstructure and Electrical Properties of Er_2O_3-Doped ZnO-Based Varistor Ceramics Prepared by High-Energy Ball Milling

The microstructure, electrical properties and density of ZnO-based varistor ceramics with different Er2O3 content prepared by high-energy ball milling （HEBM） and sintered at 800℃ were investigated. With increasing Er2O3 content, the ZnO grain size decreases due to the Er-rich phases inhibiting grain growth ; and nonlinear coefficient （ α ） decreases because of the decrease of barrier height （φB） The breakdown voltage （Eb） and density increase, whereas leakage current （IL） decreases with increasing Er2O3 content. The barrier height （φB）, donor concentration （Nd）, density of interface states （Ns） decrease and barrier width （ω） increases with increasing Er2O3 content due to acceptor effect of Er2O3 in varistor ceramics.

COMPARISON ON REFINEMENT OF IRON POWDER BY BALL MILLING ASSISTED BY DIFFERENT EXTERNAL FIELDS

The cryogenic milling and milling in conjunction with dielectric barrier discharge plasma (DBDP) have been separately set up. The combined effect of low temperature and plasma on ball milling has been investigated by examining the refinement of particle size and grain size of iron powder using scanning electron microscopy, X-ray diffraction, and small angle X-ray scattering. It was found that the mean size of iron particles could reach 104nm only after 10 hours of ball milling in conjunction with DBDP, whereas a minimum average grain size of 8.4nm was obtained by cryomilling at -20℃; however, it is difficult to refine the particle size and grain size under the same milling condition in the absence of DBDP and cryogenic temperature.

Structural and Electrochemical Characteristics of Mg_(0.94)La_(0.06)Ni Alloy Prepared by Ball Milling

The amorphous Mg_(0.94)La_(0.06)Ni alloy was synthesized by ball milling for different time at 400 r·min^(-1). Electrochemical performances of the alloy electrodes were investigated and the results show that the specimens would reach their maximum electrochemical discharge capacities at the first charge/discharge cycle. The cyclic tests and X-ray diffraction (XRD) results show that discharge capacities would decrease rapidly due to the crystallization of the amorphous and the oxidization of magnesium on the particle surface during the electrochemical charge/discharge cycling. In addition, the DTA and SEM results reveal that the thermal stabilities will be improved and the size of the alloy will be decreased with the ball-milling time. The amorphous Mg_(0.96)La_(0.04)Ni alloy prepared by ball milling for 40 h at 400 r·min^(-1) shows the best electrochemical properties.

PREPARING NANO-CRYSTALLINE La DOPED WC/Co POWDER BY HIGH ENERGY BALL MILLING

The La doped WC/Co powder was prepared by high energy ball milling. The changes of crystal structure, micrograph and defect of the powder were investigated by means of XRD (X-ray diffraction), SEM (scanning electron microscope) and DTA (differential thermal analysis). The results show that adding trace La element into carbides is effective to minish the grain size of WC/Co powder. The La doped carbides powder with grain size of 30nm can be obtained after 10h ball milling. The XRD peak of Co phase disappeared after 20h ball milling, which indicated solid solution (or secondary solid solution) of Co phase in WC phase. The La doped powder with grain size of 10nm is obtained after 30h ball milling. A peak of heat release at the temperature of 470℃ was emerged in DTA curve within the range of heating temperature, which showed that the crystal structure relaxation of the powder appeared in the process of high energy ball milling. After consolidated the La doped WC/Co alloy by high energy ball milling exhibits ultra-fine grain sizes and better mechanical properties.

Synthesis and Characterizations of Nanocrystalline WC-Co Composite Powders by a Unique Ball Milling Process

In order to explore the high efficiency of fabricating nanocrystalline WC-Co composite powders, this paper presented a unique high energy ball milling process with variable rotation rate and repeatious circulation, by which nanocrystalline WC-10Co-0.8VC-0.2Cr3C2 (wt pct) composite powders with mean grain size of 25 nm were prepared in 32 min, and the quantity of the powders for a batch was as much as 800 grams. The as-prepared powders were analyzed and characterized by chemical analysis, X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential thermal analysis (DTA). The results show that high energy ball milling with variable rotation rates and repeatious circulation could be used to produce nanocrystalline WC-Co powder composites with high efficiency. The compositions of the powders meet its specifications with low impurity content. The mean grain size decreases, lattice distortion and system energy increase with increasing the milling time. The morphology of nanocrystalline WC-Co particles displays dominantiy sphere shape and their particle sizes are all lower than 80 nm. The eutectic temperature of the nanocrystalline WC-10Co-0.8VC-0.2Cr3C2 composites is about 1280℃.

Scalable and facile synthesis of V_(2)O_(5) nanoparticles via ball milling for improved aerobic oxidative desulfurization

In recent years, transition-metal oxides(TMOs) have been long employed for aerobic oxidative desulfurization. However, the inherent bottlenecks, such as the low explosion of active sites, limit the application of bulk TMOs catalyst. In this study, V_(2)O_(5) nanoparticles with oxygen vacancies were prepared in large-scale via facile ball milling strategy with adding oxalic acid as a reducing agent. The as-prepared catalysts exhibit remarkable sulfur removal for oils with different initial S-concentrations and different substrates. Sulfur removal could reach up to 99.7%(< 2 ppm) under the optimized reaction conditions. This work provides a feasible desulfurization strategy for fuel oils.

Microwave Permeability Change of FeCo Nanocrystalline During High Energy Ball Milling

The microwave magnetic properties of the ball milled FeCo panicles were investigated as functions of ball milling time （ t ） using microwave electromagnetic parameters analysis techniques. The results show that the imaginary part of intrinsic dynamic permeability （ ui ） of the ball- milled panicles is much bigger than that of raw powders. ui strongly depends on t and exhibits several slightly damped ferromagnetic resonances. These phenomena are in qualitative agreement with the formation of the corresponding microstructure or the Aharoni ＇ s model of non-uniform exchange resonance modes. The present microwave permeabilhy behavior indicates that nanocrystalline materials with the same grain size may exhibit different properties that depend upon the microstructure, which provides a possibility for manufacturing high performance microwave absorber.

Optimization of Process Parameters for in High-Energy Ball Milling of CNTs/Al2024 Composites Through Response Surface Methodology

The mathematical models are developed to evaluate the ultimate tensile strength( UTS) and hardness of CNTs / Al2024 composites fabricated by high-energy ball milling. The effects of the preparation variables which are milling time,rotational speed,mass fraction of CNTs and ball to powder ratio on UST and hardness of CNTs / Al2024 composites are investigated. Based on the central composite design( CCD),a quadratic model is developed to correlate the fabrication variables to the UST and hardness. From the analysis of variance( ANOVA),the most influential factor on each experimental design response is identified. The optimum conditions for preparing CNTs / Al2024 composites are found as follows: 1. 53 h milling time,900 r / min rotational speed,mass fraction of CNTs 2. 87% and Ball to powder ratio 25 ∶ 1. The predicted maximum UST and hardness are 273.30 MPa and 261.36 HV,respectively. And the experimental values are 283.25 MPa and256.8 HV,respectively. It is indicated that the predicted UST and hardness after process optimization are found to agree satisfactory with the experimental values.

Effect of ball milling on hydrogen storage of Mg_3La alloy

Hydrogen storage and microstructure of ball milled Mg3La alloy were investigated by X-ray diffraction and pressure-composition-isotherm measurement. The ball milled Mg3La alloy could absorb hydrogen up to 4wt.% at 300 ℃ for the first time, along with a decomposing course. Following tests showed that the average reversible hydrogen storage capacity was 2.7wt.%. The enthalpy and entropy of dehydrogenation reaction of the decomposed ball milled Mg3La and hydrogen were calculated. XRD patterns indicated the existence of MgH2 and LaH3 in the decomposed hydride and the formation of Mg when hydrogen was desorbed. After the first hydrogenation, all the latter hydrogenation/dehydrogenation reactions could be taken place between Mg and MgH2. The ball milled Mg3La alloy exhibited better hydriding kinetics than that of the as-cast Mg3La alloy at room temperature. The kinetic curve could be well fitted by Avrami-Erofeev equation.

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

Nano-size aluminum nitride （A1N） 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 A1N 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.

Multirange Fractals in Materials: Applications to Fracture and Mechanical Alloying under Ball Milling

A new model of multirange fractals is proposed to explain the experimental results observed on the fractal dimensions of the fractured surfaces in materials. A new explanation to the Williford's multifractal curve on the relationship of fractal dimension with fracture properties in materials has been given. It shows the importance of fractorizing out the effect of fractal structure from other physical causes and separating the appropriate range of scale from multirange fractals. Mechanical alloying process under ball milling as a non-equilibrium dynamical system has been also analyzed.

Characteristics of Cr and Al Powders by High Energy Ball Milling

The variation of microstucture and phase structure of metal Cr and Al powders prepared by high energy mechanical milling was analyzed and investigated.The results show that with the continuous balling the average grain sizes of the brittle Cr powders are gradually decreased,and the diffraction peaks are widened and the peak values lower owing to the interrelation caused by both cold welding and breaking;the tough Al powders exhibit intense cold welding,and most of powders lead to adhesion to ball surface and pot wall,meanwhile,the Al powders subjected to intense deformation have led to many dislocation rings with non dislocation wind up found in the microstructure.

Preparation of CNT/AlS i10Mg composite powders by high-energy ball milling and their physical properties

This study investigated the effects of carbon nanotube （CNT） concentration on the micro-morphologies and laser absorption proper- ties of CNT/AlSi10Mg composite powders produced by high-energy ball milling. A scanning electron microscope, X-ray diffractometer, laser particle size analyzer, high-temperature synchronous thermal analyzer, and UV/VIS/NIR spectrophotometer were used for the analysis of micro- graphs, phases, granulometric parameters, thermal properties, and laser absorption properties of the composite powders, respectively. The results showed that the powders gradually changed from flake- to granule-like morphology and the average particle size sharply decreased with in- creases in milling rotational speed and milling time. Moreover, a uniform dispersion of CNTs in AlSi10Mg powders was achieved only for a CNT content of 1.5wt%. Laser absorption values of the composite powders were also observed to gradually increase with the increase of CNT concentration, and different spectra displayed characteristic absorption peaks at a wavelength of approximately 826 nm.

Formation of a FCC Al_(54)Ti_(23)C_(23) Metastable Phase by Ball Milling

The powder mixture of Al, Ti and graphite has been mechanically alloyed in a planetary ball mill.The structural evolution of as-milled powder sample has been characterized by XRD, DTA. The results show that the amorphous phase is formed first at an early milling stage, then crystallization occurs during further milling, leading to formation of a nanocrystalline fcc metastable phase. In contrast, during annealing the amorphous phase is crystallized to the equilibrium phase instead of the fcc phase. This indicates that crystallization during ball milling is different from that induced by annealing

Fabrication and microstructure of nanostructured Mg-3Ni-2MnO_(2) by ball milling in hydrogen atmosphere

Nanostructured Mg-3Ni-2MnO_(2) was synthesized by ball milling elemental powders of Mg,Ni and MnO_(2) in hydrogen atmosphere.The microstructures of the powder prepared at different milling time were analyzed by X-ray diffractometry(XRD), scanning electron microscopy(SEM)and high resolution electron microscopy(HREM).The milling time is the most key parameter impacting on the grain size and the microstructure of material.With prolonging the milling time,particle size becomes smaller and smaller.But after the ball milling time reaches about 20 h,reduction of grain size becomes slowly.When the milling time is more than 50 h,nanocrystalline fully forms.When the milling time is more than 80 h,there are more amorphous phases in materials.The average particle diameter of material is about 1μm and the grain size is 10-30 nm.

Structural Evolution of the Mn_(0.52)Sb_(0.48) Compound during High Energy Ball Milling

The structural transitions of the NiAs-type Mn0.52Sb0.48 magneto-ordered compound, ball milled to different periods, have been characterized by X-ray diffraction and DSC analysis. On the basis of lattice parameter results a structural evolution mode with three stages is proposed. In the first stage lattice parameters keep nearly unchanged with the refinement of grains and increase of lattice strain. In the second stage, microstrain shows a lowering tendency accompanying the successive decreases of grain size. The X-ray revealed internal strain is found to be strains inside the lattice, which can be relaxed with new grain formation. The change of Tc is shown to be affected by the dimension of c axis, however the overall magnetization is continuously decreased with milling, due to the disordering process occurred in milling. Correspondent disordering mechanisms have been tentatively postulated and discussed according to the changes of lattice para meters.