Particle size distribution control and related properties improvements of tungsten powders by fluidized bed jet milling

Fine grinding process of different particle size tungsten powders was carried out by fluidized bed jet milling. The results showed that the jet milling treatment caused deagglomeration of tungsten powders, which led to particles sufficient dispersion and narrow particle size distribution. Grinding gas pressure of 0.70 Mpa made the particles achieve high speed which promoted the particles collision contributing to particle dispersion and shape modification. For tungsten powder with particle size of 3 μm FSSS, a higher packing density with 5.54 g/cm³ was obtained, compared with the 3.71 g/cm³ of the original powder. For tungsten powder with particle size of 1 μm FSSS, the big agglomerates disappeared and the particle size distribution become narrower, while small aggregates about 2–3 μm still exist after the jet milling process. For tungsten powder with particle size of 5 μm and 10 μm FSSS, different medium diameter particle size and narrow particle size distribution of monodisperse tungsten powders can be produced by the optimized jet milling parameters. More important, the effective dispersion, favorable shape modification and precise classification have been achieved in the simple process.     

Processing of Cu-Fe and Cu-Fe-SiC nanocomposites by mechanical alloying

The Cu-Fe and Cu-Fe-SiC nanocomposite powders were synthesized by a two step mechanical alloying process. A supersaturated solid-solution of Cu-20 wt% Fe was prepared by ball milling of elemental powders up to 5 and 20 h and subsequently the SiC powder was added during additional 5 h milling. The dissolution of Fe into Cu matrix and the morphology of powder particles were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. It was found that the iron peaks in the XRD patterns vanish at the early stages of mechanical alloying process but the dissolution of Fe needs more milling time. Moreover, the crystallite size of the matrix decreases with increasing milling time and the crystallite size reaches a plateau with continued milling. In this regard, the addition of SiC was found to be beneficial in postponing the saturation in crystallite size refinement. Moreover, the effect of SiC on the particle size was found to be significant only if it is added at the right time. It was also found that the silicon carbide and iron particles are present after consolidation and are on the order of nanometer sizes.     

Morphological and phase evaluation of Al/15 wt.% BN nanocomposite synthesized by planetary ball mill and sintering

In this study, Al/15 wt.% BN nanocomposite was fabricated by high energy ball milling, cold compaction, and sintering process. Then the effect of milling process on the morphology change and phase evaluation was studied. The Aluminum (45 µm) and hexagonal boron nitride (70 nm) powders were milled using planetary ball mill under a pure argon atmosphere for various times of 75, 150, 300 and 600 min. The as-milled powders were consolidated at 400 MPa pressure and sintered at 600 °C for 60 min. The morphology change evaluation studied by using scanning electron microscopy (SEM) showed that the equiaxed composite powders were obtained after a short time milling process of 150 min. The steady state condition between welding and fracturing occurred by continuous milling up to 600 min. The results of X-ray diffraction patterns and differential scanning calorimetric (DSC) revealed that the BN particles completely decomposed to boron and nitrogen and dissolved in the Al matrix after 300 min of ball milling and the AlN and AlB₂ as in-situ phases were formed after sintering at temperatures above 580 °C.     

Influence of the impact sintering temperature on the structure and properties of samples from the different iron powders

The studies of the consolidation, structure and mechanical properties of samples from two types of iron powder are carried out. The coarse and less pure PZH3M2 as well as fine and purer DIAFE5000 powders were used. The samples are obtained by means of impact sintering method in the temperatures range of 500–1100 °C. The impact energy was 1200 J/cm³, and the initial deformation velocity - 6.5 m/s. Samples are obtained in the form of disks with a diameter of 25–27 mm and 9–10 mm high. For carrying out different mechanical tests the bars were cut out from disks. The tensile, compression, three-point bend of notched samples tests were carried out, as well as the Brinell hardness was measured after the corresponding processing of the bars. The characteristics of strength and plasticity of samples depending on the impact sintering temperature are determined. The polished surface of different samples and the fracture surface are investigated. It is established that the high density of samples is reached at a temperature of 600 and 700 °C respectively for fine and coarse powders. The samples obtained at these impact sintering temperatures possess rather low electrical resistivity, high strength, hardness, but the lowered plasticity. Namely, the samples from the PZH3M2 and DIAFE5000 powders sintered at the temperature of 700 °C have respectively: ultimate tensile strength - 406 and 336 MPa, yield stress - 353 and 190 MPa, contraction ratio - 26 and 78%, limit stress (at the fracture) - 501 and 933 MPa, the maximum crack tip stress – 738 and 876 MPa, the fracture energy at a bend of the notched samples - 4.8 and 51.2 J/cm³ and also Brinell hardness - 1467 and 847 MPa. The increase of the samples impact sintering temperature leads to grain growth, decrease of the samples strength and increase of their plasticity. At the same time the structure of samples from the DIAFE5000 powder is more fine-grained than at samples from the PZH3M2 powder.     

Improving the recovery of low grade coarse composite particles in porphyry copper ores

The flotation behaviour of low grade, coarse composite particles for two porphyry copper ores was studied. Different grinding times were employed to obtain size distributions for the flotation feed (d₈₀) ranging from 150 to 320 μm. Copper containing particles in the fine to intermediate size ranges were recovered in the rougher flotation stage. The rougher tailing was then screened through a 75 μm laboratory sieve. The +75 μm fraction was conditioned with a longer chain collector and floated in either normal viscosity (water) or high viscosity (glycerol–water mixture) medium. The recovery of copper was analysed on an un-sized and size-by-size basis. The recovery of coarse composite copper bearing particles was found to increase in high viscosity medium, even when the liberation of copper bearing minerals was only as low as 10%. The ability to recover these types of particles may result in a reduction in energy consumption in grinding due to the ability to achieve higher overall recovery of valuable mineral at coarse particle size distribution.     

The effects of RESS parameters on the diclofenac particle size

The RESS method was used to manufacture the fine particles of diclofenac. A reduction in particle size increases the dissolution rate of the drugs in the biological fluids and enhances the bioavailability of them in body. CO2 was used as the supercritical fluid because of its mild critical temperature (31.1 °C) and pressure (7.38 MPa). In this study, effect of extraction temperature (313–333 K), extraction pressure (14–220 MPa), spraying distance (1–10 cm), nozzle length (2–15 mm) and effective nozzle diameter (450–1700 μm) were investigated.Based on the different experimental conditions, the average particle size of diclofenac was between 10.92 and 1.33 μm. The size and morphology of the micronized diclofenac particles were monitored by scanning electron microscopy (SEM). The SEM images show a successful size reduction of virgin diclofenac particles. In all the experiments, the parameters had moderate effect on the mean particle size of the diclofenac. Also, the morphology of the processed particles was change to quasi-spherical and irregular while the virgin particles of diclofenac were irregular in shape.     

Effect of trace HA on microstructure,mechanical properties and corrosion behavior of Mg-2Zn-0.5Sr alloy

Effect of the addition of trace HA particles into Mg-2Zn-0.5Sr on microstructure, mechanical properties, and bio-corrosion behavior was investigated in comparison with pure Mg. Microstructures of the Mg-2Zn-0.5Sr-xHA composites(x = 0, 0.1 and 0.3 wt%) were characterized by optical microscopy(OM),scanning electron microscopy(SEM) equipped with energy dispersion spectroscopy(EDS) and X-ray diffraction(XRD). Results of tensile tests at room temperature show that yield strength(YS) of Mg-2Zn-0.5Sr/HA composites increases significantly, but the ultimate tensile strength(UTS) and elongation decrease with the addition of HA particles from 0 up to 0.3 wt%. Bio-corrosion behavior was investigated by immersion tests and electrochemical tests. Electrochemical tests show that corrosion potential(Ecorr)of Mg-2Zn-0.5Sr/HA composites significantly shifts toward nobler direction from-1724 to-1660 m VSCE and the corrosion current density decreases from 479.8 to 280.8 μA cm~(-2) with the addition of HA particles. Immersion tests show that average corrosion rate of Mg-2Zn-0.5Sr/HA composites decreases from11.7 to 9.1 mm/year with the addition of HA particles from 0 wt% up to 0.3 wt%. Both microstructure and mechanical properties can be attributed to grain refinement and mechanical bonding of HA particles with second phases and α-Mg matrix. Bio-corrosion behavior can be attributed to grain refinement and the formation of a stable and dense CaHPO_4 protective film due to the adsorption of Ca~(2+)on HA particles. Our analysis shows that the Mg-2Zn-0.5Sr/0.3HA with good strength and corrosion resistance can be a good material candidate for biomedical applications.     

Contact properties determination of macroscopic fine disperse glass particles via compression tests in normal direction

The paper describes the deformation behavior of spherical, dry and non-porous particles during a single particle compression test in normal direction. Therefore a compression tester was built. Industrial used soda lime glass particles with two macroscopic fine disperse sizes (d_1,50,3 = 284.30 μm and d_2,50,3 = 513.20 μm) were applied as model material to investigate the micromechanical contact behavior. In order to influence the elastic-plastic contact properties of particles, the surfaces were altered with chemical modification by means of silanization.The determination of various micromechanical contact properties (e.g. adhesion force, modulus of elasticity and contact stiffness) was carried out model-based with the contact model ‘stiff particles with soft contacts’ by means of a back-calculation.It could be shown that the model-based determination of material properties was a good alternative compared to the comprehensive tensile tests and pull-off force measurements.In addition to the gained normal force-displacement data in normal direction, the friction limits for tangential loading and rolling with the load-dependent adhesion force were model-based determined.     

Preparation of Al matrix nanocomposites by diluting the composite granules containing nano-SiCp under ultrasonic vibaration

In this work, an efficient process by diluting the nano-SiCp/Al composite granules in the molten matrix under ultrasonic vibration(UV) was developed to prepare metal matrix nano-composites(MMNCs).Millimeter-sized composite granules with high content of SiC particle(8 wt%) were specially fabricated by dry high-energy ball milling(HBM) without process control agent, and then remelted and diluted in molten Al alloy under UV. The MMNCs melt was finally squeeze cast under a squeeze pressure of 200 MPa, Microstructure of the composite granules during dry HBM was investigated, and the effect of UV on microstructure and mechanical properties of the MMNCs was discussed. The results indicate that nano-SiC particles are uniformly distributed in the nano-SiCp/Al composite granules, which are covered by vestures of pure Al. During diluting, nano-SiC particles released from the composite granules are quickly dispersed in the molten matrix by UV within 4 min. Microstructure of MMNCs is significantly refined under UV and squeeze casting, eutectic Si phase modified to fine islands with an average length of 1.4 μm. Tensile strength of the squeeze cast MMNCs with 1 wt% of nano-SiC particles is 269 MPa, which is improved by 25% compared with the A356 alloy matrix.     

Influence of size and distribution of W phase on strength and ductility of high strength Mg-5.1Zn-3.2Y-0.4Zr-0.4Ca alloy processed by indirect extrusion

A high strength Mg-5.1Zn-3.2Y-0.4Zr-0.4Ca(wt%) alloy containing W phase(Mg_3Y_2Zn_3) prepared by permanent mold direct-chill casting is indirectly extruded at 350?C and 400?C, respectively. The extruded alloys show bimodal grain structure consisting of fine dynamic recrystallized(DRXed) grains and unrecrystallized coarse regions containing fine W phase and β2' precipitates. The fragmented W phase particles induced by extrusion stimulate nucleation of DRXed grains, leading to the formation of fine DRXed grains, which are mainly distributed near the W particle bands along the extrusion direction. The alloy extruded at 350?C exhibits yield strength of 373 MPa, ultimate tensile strength of 403 MPa and elongation to failure of 5.1%. While the alloy extruded at 400?C shows lower yield strength of 332 MPa,ultimate tensile strength of 352 MPa and higher elongation to failure of 12%. The mechanical properties of the as-extruded alloys vary with the distribution and size of W phase. A higher fraction of DRXed grains is obtained due to the homogeneous distribution of micron-scale broken W phase particles in the alloy extruded at 400?C, which can lead to higher ductility. In addition, the nano-scale dynamic W phase precipitates distributed in the un DRXed regions are refined at lower extrusion temperature. The smaller size of nano-scale W phase precipitates leads to a higher fraction of un DRXed regions which contributes to higher strength of the alloy extruded at 350?C.     

Microstructure characterization,mechanical properties,compressibility and sintering behavior of Al-B4C nanocomposite powders

In the present work, Al-xB₄C nanocomposite (x = 0, 1, 2, 3, 4 and 5 in wt%, having the average B₄C size of 50 nm) were prepared using a high-energy ball mill. The milling times up to 16 h were applied. Then, the microstructural evolutions, mechanical properties, compressibility and sintering behavior of nanocomposites were investigated. The changes in powders morphology and microstructure during the milling process were characterized by laser diffraction particle size analyzer (LDA), SEM, XRD, EDS and TEM techniques. Compressibility and sintering behavior of milled powders compacted under different pressures (100–900 MPa) and at different sintering temperatures (500, 550 and 600 °C) were also studied. The pressing behavior of the nanocomposites was analyzed using linear compaction equations developed by Heckel, Panelli-Filho and Ge. The results showed the significant effects of B₄C amounts and sintering temperatures on the compressibility and sintering behavior of nanocomposites. The increase in the B₄C amount led to a decrease in both the compressibility rate and the sinterability of specimens. The maximum compression strength of 265 MPa and Vickers hardness of 165 VHN were obtained for Al-5 wt.% B₄C nanocomposite milled for 16 h followed by sintering at 600 °C.     

An experimental study of ash particles adhesion force in flue gas

In this study, experiments and analyses have been carried out to investigate the influences of denitrification and flue gas Waste Heat Recovery Systems (WHRS) on ash particles adhesion force. With use of a denitrification system, it is found that the ash particles adhesion force is strongly influenced by the mass ratio, R, of (NH₄)HSO₄ to ash. Three influencing zones are identified, i.e., little effect zone (R < 1:150), intermediate effect zone (1:150 < R < 1:60), and huge effect zone (R > 1:60). It is necessary to operate in the little effect zone in order to avoid ash deposition in the air preheater. With use of a WHRS, it is found that the ash adhesion force is strongly affected by the flue gas temperature in comparison with the Engineering Acid Dew Temperature (EADT). With decreasing temperature below the EADT, both the collected ash amount and ash adhesion force rise, and the detected particles size increases, indicating particle accumulation that improves ash collection efficiency.     

Development of NiFe-CNT and Ni3Fe-CNT nanocomposites by mechanical alloying

NiFe-CNT and Ni₃Fe-CNT nanocomposites were fabricated by high energy mechanical alloying method. X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and optical microscopy were employed for evolution of phase composition, morphology and microstructure of the powder particles. Ball milled powders were heat treated at 500 °C for 1 h to release the milling induced stresses. Bulk samples were prepared by sintering of cold pressed (300 MPa) samples at 1040 °C for 1 h. XRD patterns of powders, as-milled and after annealing at 500 °C did not show any peak related to CNTs or excess phases due to the interaction between CNTs and matrix. SEM micrographs showed that the addition of CNTs caused a reduction of powder particles size. The hardness value of as-milled NiFe and Ni₃Fe powders reach to 660 and 720 HV, respectively. According to optical microscopy evaluations, the amount and size of the porosities of the composites bulk samples decreased in comparison with matrix ones.     

Amorphization and nanocrystalline Nb3Al intermetallic formation during mechanical alloying and subsequent annealing

In this paper the formation as well as the stability of Nb₃Al intermetallic compounds from pure Nb and Al metallic powders through mechanical alloying (MA) and subsequent annealing were studied. According to this method, the mixture of powders with the proportion of Nb-25 at% Al were milled under an argon gas atmosphere in a high-energy planetary ball mill, at 7, 14, 27 and 41 h, to fabricate disordered nanocrystalline Nb₃Al. The solid solution phase transitions of MA powders before and after annealing were characterized using X-ray diffractometry (XRD). The microstructural analysis was performed using scanning electron microscopy (SEM) as well as transmission electron microscopy (TEM). The results show that in the early stages of milling, Nb(Al) solid solution was formed with a nanocrystalline structure that is transformed into the amorphous structure by further milling times. Amorphization would appear if the milling time was as long as 27 h. Partially ordered Nb₃Al intermetallic could be synthesized by annealing treatment at 850 °C for 7 h at lower milling times. The size of the crystallites after subsequent annealing was kept around 45 nm.     

Analysis of triboelectric charging of particles due to aerodynamic dispersion by a pulse of pressurised air jet

Triboelectric charging of powders causes nuisance and electrostatic discharge hazards. It is highly desirable to develop a simple method for assessing the triboelectric charging tendency of powders using a very small quantity. We explore the use of aerodynamic dispersion by a pulse of pressurised air using the disperser of Morphologi G3 as a novel application. In this device particles are dispersed by injection of a pulse of pressurised air, the dispersed particles are then analysed for size and shape analysis. The high transient air velocity inside the disperser causes collisions of sample particles with the walls, resulting in dispersion, but at the same time it could cause triboelectric charging of the particles. In this study, we analyse this process by evaluating the influence of the transient turbulent pulsed-air flow on particle impact on the walls and the resulting charge transfer. Computational Fluid Dynamics is used to calculate particle trajectory and impact velocity as a function of the inlet air pressure and particle size. Particle tracking is done using the Lagrangian approach and transient conditions. The charge transfer to particles is predicted as a function of impact velocity and number of collisions based on a charge transfer model established previously for several model particle materials. Particles experience around ten collisions at different velocities as they are dispersed and thereby acquire charges, the value of which approaches the equilibrium charge level. The number of collisions is found to be rather insensitive to particle size and pressure pulse, except for fine particles, smaller than about 30 µm. As the particle size is increased, the impact velocity decreases, but the average charge transfer per particle increases, both very rapidly. Aerodynamic dispersion by a gas pressure pulse provides an easy and quick assessment of triboelectric charging tendency of powders.     

Particle shape effects on particle size measurement for crushed waste glass

Recently, narrow particle size distributions, as measured by sieve analysis, of crushed waste glass were used as a replacement for Portland cement in concrete. Their chemical reactivity was successfully studied as a function of this measure of particle size. Differences between sieve analysis and laser diffraction measures of particle size prompted this current re-analysis. Extremely careful sieving was used to divide the crushed waste glass particles into 0–25 μm, 25–38 μm, and 63–75 μm sieve size ranges, but laser diffraction did not agree with these particle size cutoffs. We use these same materials to try and understand the discrepancies between particle size as measured by laser diffraction and sieve analysis by using X-ray computed tomography followed by spherical harmonic analysis to measure the three-dimensional particle shape and size, as well as the length (L), width (W), and thickness (T) of each particle. We show how laser diffraction and X-ray CT results, along with sieve analyses, can be quantitatively related for these crushed waste glass particles in the approximate size ranges considered. In contrast to previous speculation, the particle width W does not have to correspond closely to the sieve opening – the correspondence depends on overall particle shape. In addition, we demonstrate how many particles are needed to analyze in order to achieve stable averages and distributions of the L/W, W/T, and L/T aspect ratios, which approximately define particle shape. These results have implications for how particle size is measured and interpreted in the cement and concrete and other industries.     

Influence of processing method on the properties of hydroxyapatite nanoparticles in the presence of different citrate ion concentrations

The objective of this study was to investigate the effect of processing methods on the formation of ultra fine hydroxyapatite (HAp) nanoparticles in the presence of citrate ions and analyze their various physical properties. The addition of the citrate ions was found to reduce the size and prevent the agglomeration of HAp particles dramatically in the high gravity (HG) method compared to precipitation method. In precipitation method, the particle size reduced from 300 ± 70 nm to 90 ± 20 nm with the addition of citrate ions. In high gravity method, the particle size decreased more significantly from 80 ± 10 nm to 13 ± 5 nm with the addition of citrate ions. Furthermore, more uniform size distribution of nanoparticles was achieved in high gravity method. X-ray diffraction of nanoparticles prepared in both method exhibited slight shift of peaks to the higher angle with the addition of citric acid, indicating the incorporation of carbonate (CO₃) content in the HAp nanoparticles irrespective of the particle size. The mechanical properties of HWMPE matrix composite reinforced with nanoparticles was examined and this nanocomposite with nanoparticles prepared in high gravity method with the addition of citrate ions showed increased mechanical strength due to the considerable reduction in the particle size and higher uniformity of the particles. In vitro cellular analyses of the nanoparticle prepared in high gravity with the addition of citrate ions also displayed the most pronounced spreading of cell growth.     

Solvothermal synthesis of Ag/ZnO micro/nanostructures with different precursors for advanced photocatalytic applications

Micro/nanostructured systems based on metallic oxide (ZnO) with noble metal (Ag) on the surface (Ag/ZnO) are synthesized by solvothermal method from zinc nitrate hexahydrate (Zn(NO₃)₂·6H₂O), zinc acetate dehydrate (Zn(CH₃COO)₂·2H₂O), zinc acetylacetonate hydrate (Zn(C₅H₇O₂)₂·xH₂O) and silver nitrate (Ag(NO₃)) as precursors. In these systems, polyvinylpyrrolidone (PVP) is used as surfactant for controlling particle morphology, size and dispersion. The obtained materials are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), UV–vis diffuse reflectance spectroscopy (DRS), N₂ gas adsorption–desorption (BET) and Raman spectroscopy (RS). By XRD results, all major peaks are indexed to the hexagonal wurtzite-type structure of the ZnO and samples with noble metal, extra diffraction peaks are detected which correspond to the face-centered-cubic (fcc) structure of the metallic Ag. Depending on used precursor, different morphologies have been obtained. Mainly, ZnO prims-like rods – NRs (with 0.8 ? aspect ratio ? 3.4) – have been observed. Quasi-spherical particles of metallic Ag (with diameters between 558 ± 111 μm and 22 ± 1 nm) have been detected on the ZnO surface. Photocatalytic results (all samples studied >30% MB degradation) verify the important effect of surfactant and the viability of synthesized Ag/ZnO micro/nanocomposites for environmental applications.     

Estimation of agglomerate size of multi-walled carbon nanotubes in fluidized beds

The objective of this study was to determine hydrodynamic characteristics of multi-walled carbon nanotubes (MWCNTs) agglomerates and examine their sizes. The bed collapsing process of MWCNTs agglomerates was found to be closer to that of Geldart group C particles than group A particles. Median diameters of MWCNTs agglomerates determined by sedimentation method at initial superficial gas velocity of 0.120 and 0.190 m/s were 157 and 221 μm, respectively. The size of these MWCNTs agglomerates in fluidization state was measured by image analysis using a high speed camera. Median diameters of these MWCNTs agglomerates in freeboard were increased from 138 to 189 μm as superficial gas velocity was increased from 0.088 to 0.190 m/s at static bed height of 0.16 m. Median diameter and size distribution determined by sedimentation method fitted well with those measured using image analysis. Results were reasonable at superficial gas velocity up to 0.190 m/s.     

Numerical simulation of solid-liquid suspension in a stirred tank with a dual punched rigid-flexible impeller

The hydrodynamics of solid-liquid suspension process in a stirred tank with a dual rigid impeller, a dual rigid-flexible impeller, and a dual punched rigid-flexible impeller were investigated using computational fluid dynamics (CFD) simulation. A classical Eulerian-Eulerian approach coupled with standard k-ε turbulence model was employed to simulate solid-liquid turbulent flow in the stirred tank. The multiple reference frame (MRF) approach was used to simulate impeller rotation. The effects of impeller type, impeller speed, flexible connection piece width/length of dual rigid-flexible impeller, aperture size/ratio of dual punched rigid-flexible impeller, particle diameter, and liquid viscosity on the homogeneity degree of solid-liquid system were investigated. Results showed that the homogeneity degree of solid-liquid system increased with an increase in impeller speed. A long and wide flexible connection piece was conductive to solid particles suspension process. Larger particle diameter resulted in less homogenous distribution of solid particles. An increase in liquid viscosity was beneficial to maintain solid particles in suspension state. The optimum aperture ratio and aperture diameter were 12% and 8 mm, respectively, for solid particles suspension process. It was found that dual punched rigid-flexible impeller was more efficient in terms of solid particles suspension quality compared with dual rigid impeller and dual rigid-flexible impeller under the same power consumption.