Nanocrystalline Al/Al12(Fe,V)3Si alloy prepared by mechanical alloying: Synthesis and thermodynamic analysis

Al–Al₁₂(Fe,V)₃Si nanocrystalline alloy was fabricated by mechanical alloying (MA) of Al–11.6Fe–1.3V–2.3Si (wt.%) powder mixture followed by a suitable subsequent annealing process. Structural changes of powder particles during the MA were investigated by X-ray diffraction (XRD). Microstructure of powder particles were characterized using scanning electron microscopy (SEM). Differential scanning calorimeter (DSC) was used to study thermal behavior of the as-milled product. A thermodynamic analysis of the process was performed using the extended Miedema model. This analysis showed that in the Al–11.6Fe–1.3V–2.3Si powder mixture, the thermodynamic driving force for solid solution formation is greater than that for amorphous phase formation. XRD results showed that no intermetallic phase is formed by MA alone. Microstructure of the powder after 60 h of MA consisted of a nanostructured Al-based solid solution, with a crystallite size of 19 nm. After annealing of the as-milled powder at 550 °C for 30 min, the Al₁₂(Fe,V)₃Si intermetallic phase precipitated in the Al matrix. The final alloy obtained by MA and subsequent annealing had a crystallite size of 49 nm and showed a high microhardness value of 249 HV which is higher than that reported for similar alloy obtained by melt spinning and subsequent milling.     

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.     

X-ray line profile analysis of the ball-milled Fe–30Co alloy

This work deals with the microstructural properties of the Fe–30Co alloy prepared by ball milling of elemental iron and cobalt powders. The obtained mixed powder has been characterized by means of scanning electron microscope, X-ray microanalysis, laser diffraction, X-ray diffraction and microhardness measurements. X-ray line profile analysis based on the Rietveld method and adopting two different models has been used for the microstructural study. The refinement of the X-ray patterns shows that after 3 h of high energy milling the Fe(Co) is formed. The obtained Fe(Co) solid solution is characterized by body centered cubic structure with a lattice parameter a = 0.28564 ± 0.00004 nm and an ellipsoidal crystallite and microstrain field. The dissolution of cobalt in iron matrix is accompanied by the compression of the crystalline lattice by 0.37%. The progress of milling process produces an increase of the Debye–Waller factor and the dislocation density leading to the hardening of the powder. The variation of microhardness with milling time shows a change in hardening mechanisms.     

Simultaneous carbothermic reduction of iron and titanium oxides to produce an iron-based composite by mechanically activated sintering method

In this research, for the first time, Fe–TiC nano-crystalline composite was produced via simultaneous reduction of iron and titanium oxides by petrocoke. Powder mixture of Fe₂O₃/TiO₂/petrocoke was mechanically activated in a high-energy ball mill at different times. X-ray diffraction method (XRD) and Scanning Electron Microscopy (SEM) were used to characterize the milled powders. The results showed that new phases were not formed during milling, even after 20 h of milling. However, crystallite size and lattice strain of hematite were remarkably decreased and increased, respectively. Thermogravimetry and Differential Thermal Analysis (TG–DTA) were done on 0, 10 and 20 h mechanically activated powders. These experiments showed a substantial decrease in reduction temperature of iron and titanium oxides as a result of mechanical activation. Then, the powders were cold compacted and sintered at 1200 °C in argon atmosphere for 1 h. XRD results of 20 h milled samples demonstrated that, in this condition, iron oxide was completely reduced to nano-crystalline iron and titanium dioxide was reduced to nano-crystalline titanium carbide and Fe–TiC nano-crystalline composite was successfully formed.     

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.     

Fabrication of Al2O3–20 vol.% Al nanocomposite powders using high energy milling and their sinterability

In this study, alumina-based matrix nanocomposite powders reinforced with Al particles were fabricated and investigated. The sinterability of the prepared nanocomposite powder at different firing temperature was also conducted. Their mechanical properties in terms of hardness and toughness were tested. Alumina and aluminum powder mixtures were milled in a planetary ball mill for various times up to 30 h in order to produce Al₂O₃–20% Al nanocomposite. The phase composition, morphological and microstructural changes during mechanical milling of the nanocomposite particles were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) techniques, respectively. The crystallite size and internal strain were evaluated by XRD patterns using Scherrer methods.A uniform distribution of the Al reinforcement in the Al₂O₃ matrix was successfully obtained after milling the powders. The results revealed that there was no any sign of phase changes during the milling. The crystal size decreased with the prolongation of milling times, while the internal strain increased. A simple model is presented to illustrate the mechanical alloying of a ductile–brittle component system. A competition between the cold welding mechanism and the fracturing mechanism were found during powder milling and finally the above two mechanisms reached an equilibrium. The maximum relative density was obtained at 1500 °C. The harness of the sintered composite was decreased while the fracture toughness was improved after addition Al into alumina.     

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.     

Study on preparation and mechanical property of nanocrystalline NiAl intermetallic

Nanocrystalline NiAl materials were fabricated using mechanical alloying and hot-pressing sintering technique. The crystal structural and microstructure of milled powders during mechanical alloying, and the microstructure and mechanical properties of bulk NiAl intermetallic were characterized. The results show that B2 ordered nanocrystalline NiAl powders were successfully synthesized by solid-state diffusion via the gradual exothermic reaction mechanism during mechanical alloying. Scanning electron microscope image confirmed that the powder particles were flat and flake shape in the early stage of milling, but changed to a spherical shape with the crystallite size about 30 nm after the milling. After sintering, the crystal structure of nanocrystalline NiAl intermetallic was assigned to B2 order NiAl phase with the average crystallite size about 100 nm. The nanocrystalline NiAl intermetallic exhibited prominent room temperature compressive properties, such as the true ultimate compressive strength and the fracture strain were 2143 MPa and 32.2%, respectively. The appearances of vein-like patterns on the fracture surface of NiAl intermetallic materials indicated that the fracture mechanism could be characterized as ductile fracture. It can be concluded that higher sintering density and nanocrystalline of NiAl intermetallic were benefited for the improvement of mechanical properties.     

A study on the mechanochemical behavior of TiO2–Al–Si system to produce Ti5Si3–Al2O3 nanocomposite

In the present study Ti₅Si₃–Al₂O₃ nanocomposite was synthesized by a displacement reaction between Al and TiO₂ in ball milling of TiO₂, Al and Si powders. The effect of milling time and heat treatment temperatures were also investigated. The structural changes of powder particles during mechanical alloying were investigated by X-ray diffraction (XRD). Morphology and microstructure of powders were characterized by scanning electron microscopy (SEM). It was found that after 10 h of MA, the reaction between Al and TiO₂ initiated in a gradual mode and after about 45 h of milling, the reaction was successfully completed. The final product consisted of Ti₅Si₃ intermetallic compound with a crystallite size of 13 nm and amorphous Al₂O₃. Heat treatment of this structure at 1050 °C led to the crystallization of Al₂O₃ and ordering of Ti₅Si₃. The crystallite size of Ti₅Si₃ and Al₂O₃ after annealing at 1050 °C for 1 h remained in nanometer scale. So the final product appeared to be stable upon annealing.     

Structural and microstructural phase evolution during mechano-synthesis of nanocrystalline/amorphous CuAlMn alloy powders

The formation mechanism of Cu–11.5Al–4Mn alloys by mechanical alloying (MA) of pure elemental powders was investigated. During milling, the powder sampling was conducted at predetermined intervals from 1 h to 96 h. The quantitative phase analyses were done by X-ray diffraction and the particles size and morphology were studied by scanning electron microscopy. Furthermore, the microstructure investigation and phase identification were done by transmission electron microscopy. Concerning the results, the nanocrystalline Cu solid solution were formed at short milling times and, by milling evolution, the austenite-to-martensite (2H) phase transformation occurred. Moreover, the formation of considerable amount of amorphous phase and its partial transformation to crystalline phases during the milling process were revealed. It was also found that, by milling development, the powder morphology changes from lamellar to semi-spherical and their size initially increases, then reduces and afterward re-increases.     

Effect of ball milling on the physical and mechanical properties of the nanostructured Co–Cr–Mo powders

In the present study, Co-based machining chips (P1) and Co-based atomized alloy (P2) has been processed through planetary ball mill in order to obtain nanostructured materials and also to comprise some their physical and mechanical properties. The processed powders were investigated by X-ray diffraction technique in order to determine several microstructure parameters including phase fractions, the crystallite size and dislocation density. In addition, hardness and morphological changes of the powders were investigated by scanning electron microscopy and microhardness measurements. The results revealed that with increasing milling time, the FCC phase peaks gradually disappeared indicating the FCC to HCP phase transformation. The P1 powder has a lower value of the crystallite size and higher degree of dislocation density and microhardness than that of the P2 powder. The morphological and particle size investigation showed the role of initial HCP phase and chemical composition on the final processed powders. In addition results showed that in the first step of milling the crystallite size for two powders reach to a nanometer size and after 12 h of milling the crystallite size decreases to approximately 27 and 33 nm for P1 and P2 powders, respectively.     

Effect of cup and ball types on alumina–tungsten carbide nanocomposite powder synthesized by mechanical alloying

Alumina-based nanocomposite powders with tungsten carbides particulates were synthesized by ball milling WO₃, Al and graphite powders. X-ray Diffraction (XRD) was used to characterize the milled and annealed powders. Microstructures of milled powders were studied by Transmission Electron Microscopy (TEM). Results showed that Al₂O₃–W₂C composite formed after 5 h of milling with major amount of un-reacted W in stainless steel cup. The remained W was decreased to minor amount by increasing carbon content up to 10 wt.%. When milled with ZrO₂ cup and balls, Al₂O₃–W₂C composite was completely synthesized after 20 h of milling with the major impurity of ZrO₂. In the case of stainless steel cup and balls with 10 wt.% carbon, Fe impurity after 5 h of milling (maximum 0.09 wt.%) was removed from the powder by leaching in 3HCl·HNO₃ solution. The mean grain size of the powder milled for 5 h was less than 60 nm. The powder preserved its nanocrystalline nature after annealing at 800 °C.     

X-ray diffraction and Mössbauer spectrometry studies of the mechanically alloyed Fe–6P–1.7C powders

Nanostructured Fe–6P–1.7C powders were obtained by mechanical alloying in a planetary ball mill. Morphological, microstructural and structural changes during the milling process were followed by scanning electron microscopy, X-ray diffraction and ⁵⁷Fe Mössbauer spectrometry. The crystallite size refinement to the nanometer scale (5–8) nm is accompanied by an increase in the internal strain. The nanocrystalline structure distortion is evidenced by the lattice parameter changes of the milling products. The hexagonal Fe₂P phosphide is formed within 6 h of milling, while the tetragonal Fe₃P and orthorhombic Fe₃C phases appear after 12 h of milling. A mixture of Fe₃P phosphide, Fe₃C carbide and α-Fe(C, P) solid solution is obtained on further milling time.     

Fabrication and evaluation of oxidation resistance performance of open-celled Fe(Al) foam by space-holder technique

First, fabrication of Fe(Al) open-cell foams by using space-holder technique, in which NaCl powder and polyester resin were utilized as space holder and binder, was investigated. Fe(Al) powder were prepared via mechanical alloying method after 5 h milling process. Then, the influences of fabrication parameters, alloying element Al content, time of milling process, sintering temperature and soaked time on the oxidation resistance performance of foam specimens at 800 °C were mainly studied. The experimental results exhibit that alloying with 2 wt.% Al resulted in acceleration of the oxidation rate of foam samples, additionally, alloying with 4 wt.% Al had a little positive effect on oxidation rate at 800 °C. However, the oxidation resistance of the 10 wt.% Al-containing sample greatly improves compared to pure Fe. In addition, the oxidation resistance performance of prepared foam was improved by increasing the milling time up to 15 h, and followed by a decrease gradually. The increase of sintering temperature and the prolongation of soaked time to 1100 °C and 90 min, respectively had significant positive effect on the oxidation resistance.     

Improvement of magnetic properties of nanostructured Ni79Fe16Mo5 alloyed powders by a suitable heat treatment

The supermalloy (Ni₇₉Fe₁₆Mo₅) nanostructured powder with average crystallite size of about 8 nm was prepared by high energy milling. The obtained powders were characterized by X-ray diffraction, scanning electron microscopy, differential scanning calorimetry and vibration sample magnetometer. The results showed that the coercivity and the saturation magnetization reach about 8 Oe and 75 emu/g at 96 h and become approximately 1 Oe and 85 emu/g after a suitable heat treatment, respectively. The magnetic measurements confirmed that the supermalloy soft magnetic nanostructure powder was produced by mechanical alloying followed by a post heat treatment. The results revealed that a small amount of Mo element remain in the system up to 96 h due to (i) high fusion temperature, T_f = 2893 K, (ii) high mechanical hardness, (iii) low solubility of Mo into Ni at low temperatures in mechanical alloying conditions.     

Structure and properties of ductile CuAlMn shape memory alloy synthesized by mechanical alloying and powder metallurgy

A ductile Cu–Al–Mn–Ti–B shape memory alloy with high fatigue strength has been prepared via mechanical alloying and powder metallurgy. With increasing milling time, the size of the crystallite grains decreases. Cu diffraction pattern appeared only after milling at a speed of 300 rpm for 25 h. The single phase CuAlMnTiB solid solution powder after 35 h milling was hot-pressed and extruded to form the final alloy. The quenched alloy had a single β phase at room temperature and its yield strength, maximum strength and strain were measured to be 390 MPa, 1015 MPa and 14.4%, respectively. The aged alloy showed a martensite structure at room temperature and had a shape memory recovery of 92% after 120 cycles.     

Mechanical alloying and sintering of nanostructured TiO2 reinforced copper composite and its characterization

Mechanical alloying is a suitable method for producing copper based composites. Cu–TiO₂ composite was fabricated using high energy ball milling and conventional consolidation. Ball milling was performed at different milling durations (0–24 h) to investigate the effects of the milling time on the formation and properties of produced nanostructured Cu–TiO₂ composites. The amount of the TiO₂ in the final composition of the composite assumed to be 0, 1, 3, 5 and 7 wt%. The milled composite powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy to investigate the effects of the milling time on the formation of the composite and its properties. Also hardness, density and electrical conductivity of the sintered specimen were measured. High energy ball milling causes a high density of defects in the powders. Thus the Cu crystallite size decreases, generally to less than 50 nm. The maximum hardness value (105 HV) of the sintered compacts belongs to Cu–5 wt%TiO₂ which has been milled for 12 h.     

Synthesis, characterization and annealing of mechanically alloyed nanostructured FeAl powder

Elemental powders of Fe and Al were mechanically alloyed using a high energy rate ball mill. A nanostructure disordered Fe(Al) solid solution was formed at an early stage. After 28 h of milling, it was found that the Fe(Al) solid solution was transformed into an ordered FeAl phase. During the entire ball milling process, the elemental phase co-existed with the alloyed phase. Ball milling was performed under toluene to minimise atmospheric contamination. Ball milled powders were subsequently annealed to induce more ordering. Phase transformation and structural changes during mechanical alloying (MEA) and subsequent annealing were investigated by X-ray diffraction (XRD). Scanning electron microscope (SEM) was employed to examine the morphology of the powders and to measure the powder particle size. Energy dispersive spectroscopy (EDS) was utilised to examine the composition of mechanically alloyed powder particles. XRD and EDS were also employed to examine the atmospheric and milling media contamination. Phase transformation at elevated temperatures was examined by differential scanning calorimeter (DSC). The crystallite size obtained after 28 h of milling time was around 18 nm. Ordering was characterised by small reduction in crystallite size while large reduction was observed during disordering. Micro hardness was influenced by Crystallite size and structural transformation.     

Mechanical alloying and spark plasma sintering of CoCrFeNiMnAl high-entropy alloy

An equiatomic CoCrFeNiMnAl high-entropy alloy was synthesized by mechanical alloying, and alloying behaviors, microstructure and annealing behaviors were investigated. It was found that a solid solution with refined microstructure of 20 nm in grain size could be obtained after 30 h milling. As-milled powder transformed into a face-centered cubic phase above 500 °C. The as-milled powder was subsequently consolidated by spark plasma sintering at 800 °C, BCC phase and FCC phase coexisted in the consolidated HEA, which had excellent properties in Vickers hardness of 662 HV and compressive strength of 2142 MPa.     

Combustion characteristics of the heat pellet prepared from the Fe powders obtained by spray pyrolysis

Fe powders for thermal batteries were prepared by reduction of iron oxide powders obtained by spray pyrolysis. The iron oxide powders prepared by spray pyrolysis had fine size, spherical shape and high surface area. The morphologies of the Fe powders were affected by the preparation temperatures of the iron oxide powders. The Fe powders obtained from the iron oxide powders prepared by spray pyrolysis at 900 and 1000 °C had slightly aggregated structure of the primary powders with several microns sizes. The powders had pure Fe phases at reducing temperatures between 600 and 800 °C. The heat pellets with diameter of 18.2 mm were prepared using Fe powders and potassium perchlorate (KClO₄). The porosity of the prepared heat pellet was about 40%. The break strength of the heat pellet was 0.9 kgf. The ignition sensitivity of the heat pellet was 4 W. The maximum burn rate of the heat pellet obtained from the Fe powders were 8.6 cm s^?1.