Ball milling of Co70 Fe8Si9B13 amorphous ribbon,crystallized ribbon and a mixture of pure crystalline powders

Co₇₀ Fe₈ Si₉B₁₃ amorphous ribbon, crystallized ribbon and a mixture of pure crystalline powders were mechanically alloyed by milling and nanocrystalline structures were obtained. The structural changes were monitored By X-ray diffraction and differential scanning calorimetry measurements. The thermal behaviour on heating the alloys prepared by ball milling was studied and the influence of the high-energy ball milling on the resulting phases was found.     

Sintering behavior of mechanically alloyed Ti-48Al-2Nb aluminides

Ti-Al intermetallics have been produced using mechanical alloying technique. A composition of Ti-48Al-2Nb at % powders was mechanically alloyed for various durations of 20, 40, 60, 80 and 100 h. At the early stages of milling, a Ti (Al) solid solution is formed, on further milling the formation of amorphous phase occurs. Traces of TiAl and Ti₃Al were formed with major Ti and Al phases after milling at 40 h and beyond. When further milled, phases of intermetallic compounds like TiAl and Ti₃Al were formed after 80 hours of milling and they also found in 100 h milled powders. The powders milled for different durations were sintered at 785°C in vacuum. The mechanically alloyed powders as well as the sintered compacts were characterized by XRD, FESEM and DTA to determine the phases, crystallite size, microstructures and the influence of sintering over mechanical alloying.     

Electrocatalytic properties of mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo alloy powders

Mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo (nominal compositions) alloy powders were produced by milling of pure elemental powders. Mechanically alloyed powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. MA powder specimens were tested electrollitically in a 30% KOH aqueous solution at 298 K. X-ray diffraction analysis and transmission electron microscopy of milled powders showed the presence of two phases, an fcc solid solution and intermetallic compounds of Ni or Co with Mo. These phases showed a nanometric size. The linear sweep voltammograms confirmed also the presence of two phases in both mechanically alloyed alloy powders. The Co-20wt%Ni-10wt%Mo alloy powders showed the best electrocatalytic activity for hydrogen evolution reaction.     

Characteristics of the mechanically-alloyed Ni60Ti40 amorphous powders during mechanical milling in different atmospheres

Mechanically alloyed Ni₆₀Ti₄₀ amorphous powders were further milled in argon, nitrogen and oxygen atmospheres. X-ray diffraction, differential scanning calorimetry and transmission electron microscopy analyses were made to investigate the structural changes during each process. No distinguishable structural changes during further milling of the amorphous powders in argon or nitrogen atmospheres were observed. However, in an oxygen atmosphere, the amorphous phase was crystallized into intermetallic compounds and was accompanied by the occurrence of titanium oxides in the initial stage. On further milling in an oxygen atmosphere, the intermetallic compounds decomposed and only the nickel saturation solution and titanium oxides remained. A thermodynamic explanation of the crystallization and decomposition has been proposed.     

Effect of ball milling time on the structural characteristics and mechanical properties of nano-sized Y2O3 particle reinforced aluminum matrix composites produced by powder metallurgy route

Mechanical milling presents an effective solution in producing a homogenous structure for composites. The present study focused on the production of 0.5 wt% yttria nanoparticle reinforced 7075 aluminum alloy composite in order to examine the effects of yttria dispersion and interfacial bonding by ball milling technique. The 7075 aluminum alloy powders and yttria were mechanically alloyed with different milling times. The milled composites powders were then consolidated with the help of hot pressing. Hardness, density, and tensile tests were carried out for characterizing the mechanical properties of the composite. The milled powder and the microstructural evolution of the composites were analyzed utilizing scanning and transmission electron microscopy. A striking enhancement of 164% and 90% in hardness and ultimate tensile strength, respectively, were found compared with the reference 7075 aluminum alloy fabricated with the same producing history. The origins of the observed increase in hardness and strength were discussed within the strengthening mechanisms' framework.     

Thermal stability and phase formation of mechanically alloyed Ti-Al-Si-C powders

Two quarternary Ti-Al-Si-C powder mixtures, 55Ti-27Al-12Si-6C and 55Ti-36Al-6Si-3C, were mechanically alloyed. The as-alloyed and heated powders have been characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and differential scanning calorimetry (DSC). XRD patterns showed diffuse halos of amorphous like phase for 20-40 h milled powders, but TEM examinations demonstrated that the 40 h milled powders were mainly composed of Ti solid solutions, with some amount of amorphous phase. SEM observations displayed that the lamellar structures of Ti and Al formed at the early stage of milling process subsequently led to the formation of nano- or sub-micrometer particles of homogeneous composition after prolonged milling to 40 h. It is deduced that the solid-stated reaction by inter-diffusion of components should be responsible for phase formation during mechanical alloying. DSC curves of the 40 h milled powders exhibited two sharp exothermal peaks, and the investigation on thermal stability of the 40 h milled powders indicated that Ti₅Si₃ was first formed at lower temperature, followed by Al₂Ti₄C₂and TiC at intermediate temperature (820°C), and these phases were stable at elevated temperatures. These results raise the possibility of synthesizing TiAl-based composite with titanium silicides and titanium carbides as reinforcements by proper selection of powder compositions.     

Microstructural and mechanical characterisation of ODS ferritic alloys produced by mechanical alloying and spark plasma sintering

Abstract

Powders with nominal composition Fe–14Cr–2W–0·4Ti were mechanically alloyed (MA) with Y₂O₃ in a planetary ball mill at two different rotational speeds. Consolidation of the as milled powders was performed by spark plasma sintering (SPS). As milled powders showed a highly deformed microstructure with elongated nanometre grains and, depending upon the rotational speed, different stages of the nanocluster evolution were observed to be produced. In the case of consolidated materials, grain growth occurred during the SPS process and it was possible to observe the influence of the MA parameters, with larger and more homogeneously distributed grains at the higher rotational speed. Additionally, Ti was observed to be incorporated to the nanoclusters after SPS, indicating a further step in their evolution during consolidation. The mechanical behaviour of the SPS compacts was evaluated by tensile and small punch testing also showing the influence of the MA parameters in the material behaviour.     

Mechanical Alloying of Ti50Al50 Powders and Their Consolidated Properties

Elemental powder mixtures of 50Ti-50Al (at.%) were mechanically alloyed via various ball milling methods. The microstructural evolution during the milling indicates that the mechanical alloying behavior is strongly affected by milling methods, and horizontal ball milling is most effective for producing homogeneous metastable powders. The mechanically alloyed powders were consolidated by vacuum hot pressing followed by homogeneous annealing. Compression testing results showed that the annealed specimens still retain fine grains and have a good combination of fracture strength and ductility, as compared to cast specimens of the same alloy.     

Crystalline – Amorphous AA4048 – Al60Nb40 composites processed by mechanical alloying and powder compaction

Commercial crystalline AA4048 powders and mechanically alloyed amorphous Al₆₀Nb₄₀ (at.%) powders were used for fabrication of crystalline-amorphous composites containing 10, 20 and 30?vol% of amorphous phase. High pressure high temperature technique was used for powders compaction. The applied pressure was 7.7?GPa and temperature was in the range 600–1000?°C. The powders and bulk samples were characterized by structural investigations (X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, X-ray fluorescence spectroscopy), hardness and microhardness tests and measurements of density. The obtained sinters revealed relative density above 98.7%. The amorphous component was observed as agglomerates or as single particles surrounding the grains of crystalline AA4048 phase. The crystallization of amorphous phase was not observed. Simultaneously, up to 2.5?wt% of Fe was detected as impurity from milling media. Significant increase of hardness was observed, from 226 to 288HB, resulting from the presence of amorphous component which prevent from cracks propagation during deformation.     

Formation of Magnesium Silicide by Mechanical Alloying

Elemental Mg and Si powders were mechanically alloyed in a planetary ball mill. The formation of magnesium silicide as well as the formation of magnesium oxide and hydride in the milled powders was studied in detail by X-ray diffraction and scanning differential calorimetry. It was found that direct formation of the magnesium silicide, Mg₂Si, occurred after 10 hours of milling and the content of Mg₂Si increased with increasing the milling duration. The activation energy for the formation of Mg₂Si was calculated by the Kissinger approach to be 215 kJ/mol. Besides oxidizing and hydrizing of Mg by decomposed organic additives during mechanical alloying, an increased contamination of powders from steel and alumina milling tools with increasing milling duration was detected. A short milling duration followed by a thermal treatment was thus suggested to synthesize magnesium silicide.     

Synthesis of nanocrystalline/quasicrystalline Mg32(Al,Zn)49 by melt spinning and mechanical milling

In the present investigation we have made an attempt to synthesize T-Mg₃₂(Al,Zn)₄₉ Frank Kasper phase and investigate the mechanical properties of the T-Phase in micro and nano scale. Single T-Phase (bcc, a = 1.42 nm) has been prepared by conventional casting with a proper combination of flux in order to avoid the loss of magnesium from the melt. Chemical analysis by energy dispersive X-ray microanalysis system attached to scanning electron microscope has confirmed the desired composition for T-phase. The as-cast material was then rapidly solidified by melt spinning and mechanically milled using a high-energy ball mill. The samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction techniques. The rapidly solidified foils showed the presence of mostly nanoquasicrystalline phases coexisting with a minute amount of crystalline phases in the thin region where the cooling rate is expected to be high. The dark field imaging in electron microscopy clearly confirms the existence of nano phases. Mechanically milled powder exhibited the evolution of nanophases at higher milling time. Microhardness measurement at low load was carried out in both the as-cast and nanophase materials in order to understand the influence of nanophases on the mode of deformation and cracking at low load.     

Improvement of sinterability of gadolinia-doped ceria via a high-energy ball milling process

High-energy ball milling process has been applied to gadolinia-doped ceria system. The sinterability of gadolinia-doped ceria was significantly enhanced by the high-energy ball milling process. A comparison was also made of the sintering behavior of milled powders doped with gallia as a sintering aid. Dense Ce_0.8Gd_0.2O_1.9 ceramics with 97% of the theoretical density could be obtained by sintering the milled mixture with 0.5 mol% Ga₂O₃ addition at 1,250 °C for 5 h.     

Aluminium based composites strengthened with metallic amorphous phase or ceramic (Al2O3) particles

Two methods were used to obtain amorphous aluminium alloy powder: gas atomization and melt spinning. The sprayed powder contained only a small amount of the amorphous phase and therefore bulk composites were prepared by hot pressing of aluminium powder with the 10% addition of ball milled melt spun ribbons of the Al₈₄Ni₆V₅Zr₅ alloy (numbers indicate at.%). The properties were compared with those of a composite containing a 10% addition of Al₂O₃ ceramic particles. Additionally, a composite based on 2618A Al alloy was prepared with the addition of the Al₈₄Ni₆V₅Zr₅ powder from the ribbons used as the strengthening phase. X-ray studies confirmed the presence of the amorphous phase with a small amount of aluminium solid solution in the melt spun ribbons. Differential Scanning Calorimetry (DSC) studies showed the start of the crystallization process of the amorphous ribbons at 437 °C. The composite samples were obtained in the process of uniaxial hot pressing in a vacuum at 380 °C, below the crystallization temperature of the amorphous phase. A uniform distribution of both metallic and ceramic strengthening phases was observed in the composites. The hardness of all the prepared composites was comparable and amounted to approximately 50 HV for those with the Al matrix and 120 HV for the ones with the 2618A alloy matrix. The composites showed a higher yield stress than the hot pressed aluminium or 2618A alloy. Scanning Electron Microscopy (SEM) studies after compression tests revealed that the propagation of cracks in the composites strengthened with the amorphous phase shows a different character than these with ceramic particles. In the composite strengthened with the Al₂O₃ particles cracks have the tendency to propagate at the interfaces of Al/ceramic particles more often than at the amorphous/Al interfaces.     

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti55C45 bulk material

We employed a high-energy ball mill for the synthesis of nanograined Ti₅₅C₄₅ 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 200 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^1/2, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed.     

High temperature magnetic properties of mechanically alloyed Fe–Zr powder

We report the preparation and characterization of amorphous/non-equilibrium solid solution Fe_100 − xZr_x (x = 20–35) alloys by mechanical alloying process. The microstructure and magnetic properties of milled powders have been studied as a function of Zr substitution. The effective magnetic moment of as-milled powders decreases as concentration of Zr is increased. Thermomagnetization measurements confirmed that the Fe₈₀Zr₂₀ sample exhibits two clear magnetic phase transitions due to the co-existence of an amorphous phase and a Fe rich non-equilibrium solid solution. All the other samples exhibiting an amorphous structure showed a single magnetic phase transition with Curie temperature of ~ 570 °C,which did not vary much with different composition. The Curie temperature of the mechanically alloyed powders is noticeably higher than those of melt-spun amorphous ribbons.     

Synthesis of LaB<Subscript>6</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposite powders via ball milling-assisted annealing

In this study, LaB₆–Al₂O₃ nanocomposite powders were synthesized via ball milling-assisted annealing process starting from La₂O₃–B₂O₃–Al powder blends. High-energy ball milling was conducted at various durations (0, 3, 6 and 9 h). Then, the milled powders were annealed at 1200 °C for 3 h under Ar atmosphere in order to obtain LaB₆ and Al₂O₃ phases as reaction products. X-ray diffractometry (XRD), scanning electron microscopy/energy-dispersive spectrometry (SEM/EDS) and transmission electron microscopy (TEM) techniques were utilized to carry out microstructural characterization of the powders. No reaction between the reactants was observed in the XRD patterns of the milled powders, indicating that high-energy ball milling did not trigger any chemical reactions even after milling for 9 h. LaAlO₃ and LaBO₃ phases existed in the annealed powders which were milled for 0, 3 and 6 h. LaBO₃ phase was removed after HCl leaching. 9-h milled and annealed powders did not exhibit any undesired phases such as LaAlO₃ and LaBO₃ after leaching step, and pure nanocrystalline LaB₆–Al₂O₃ composite powders were successfully obtained. TEM analyses revealed that very fine LaB₆ particles (~?100 nm) were embedded in coarse Al₂O₃ (~?500 nm) particles.     

Ultrafast synthesis of the nanostructured Al59Cu25.5Fe12.5B3 quasicrystalline and crystalline phases by high-energy ball milling: Microhardness,electrical resistivity,and solar cell absorptance studies

In this study, the Al₅₉Cu_25.5Fe_12.5B₃ nanoquasicrystalline alloy and related crystalline phases were synthesized through mechanical alloying using a high-energy ball milling and consolidated by a cold isostatic pressing apparatus. This paper focuses on the synthesis, structural and microstructural evolutions, thermal stability, microhardness, and electrical and optical properties of the Al₅₉Cu_25.5Fe_12.5B₃ nanoquasicrystalline alloy for solar selective absorber usages. The structural evolutions of the mechanically alloyed and heat-treated AlCuFeB powders were investigated by X-ray diffractometry. Accordingly, the effect of milling time and heat treatment on the formation of quasicrystalline and related crystalline phases were studied in the AlCuFeB alloy system. The microstructure, morphology, and chemical microanalysis of the un-milled and as-milled powders were examined by field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. The composition of the as-milled AlCuFeB powders was estimated employing inductively coupled plasma-atomic emission spectroscopy. The thermal stability of the AlCuFeB powders was recorded by differential thermal analysis, and the weight gain of the particles during annealing was investigated through thermogravimetric analysis. The nanostructured Al₅₉Cu_25.5Fe_12.5B₃ stable quasicrystalline phase and crystalline Al(Cu,Fe) solid-solution were synthesized by the ultrafast milling procedure in 1 h. The rationale behind using the term ultrafast synthesis is to synthesize the QC i-phase only by the high-energy ball milling procedure in short-term ball milling without subsequent annealing treatment. However, the single quasicrystalline phase could not be obtained even after the annealing treatment. The quasicrystalline size was calculated by the Williamson–Hall method and optimized by the Rietveld refinement procedure, and it was found that the size is varied between 53 and 61 nm. Furthermore, the particle size distribution of the as-milled AlCuFeB powders was measured using laser static light scattering, which ranges from 0.1 to 50 μm. The microhardness of the consolidated as-milled and heat-treated samples was estimated utilizing the Vickers microhardness indenter. At the same time, their electrical resistivity was assessed by the four-point probe method at room temperature. The spectral analyses of absorption on the consolidated as-milled samples were carried out in the ultraviolet, visible, and near-infrared regions. It was found that the presence of the quasicrystalline phase in the AlCuFeB alloy prominently improves the microhardness, electrical resistivity, and particularly sunlight absorptance.     

Hydriding processes of Mg and Zr alloys by reactive milling

Mechanically alloyed Mg₂Ni/Ni nano-composite and Zr₅₅Cu₃₀Ni₅Al₁₀ amorphous powders were hydrogen charged at constant pressure under ball milling. While the Mg-based samples were able to absorb large amount of hydrogen under static conditions, and from the very onset of the mechanical treatment, an incubation milling period was needed for the hydrogen activation in the case of the amorphous sample. A progressively decreasing rate characterizes the process kinetics in the case of Mg₂Ni/Ni, whereas a self increasing sigmoid trend was observed for the multicomponent Zr alloy, which showed structural demixing phenomena in the absorption course. Irrespective of the system, the maximum absorption rate was strongly dependent on the milling intensity (Watt·g^-1). The hydriding rate (mole·g^-1s^-1) and the mechanochemical yield (mole·Joule^-1) were used to compare the processes on an absolute scale. In the case of Mg-based alloy, comparison was also made between mechanically induced and thermally (static) activated hydriding processes. Attempt was also made to work out the hydrogen atoms absorbed at the ball-hit event.     

Formation of quasicrystals in ball-milled amorphous Zr-Ti-Nb-Cu-Ni-Al alloys with different Nb content

In order to investigate the effect of the preparation technique on quasicrystal formation, amorphous (Zr_0.585Ti_0.082Cu_0.142Ni_0.114Al_0.077)_100?x Nb _x alloys with x = 2.5 and 5 at.% were produced by melt spinning and by ball milling of crystalline intermetallic compounds. The calorimetric and microstructure investigations revealed striking similarities between the differently synthesized samples. All the samples are characterized by a two-step crystallization process in which the first crystallization product does not depend on the way of preparation. In fact, the same metastable nanoscale quasicrystalline phase has been obtained by partial devitrification of ball-milled powders as well as of melt-spun ribbons. This demonstrates that ball milling is an alternative processing route to rapid solidification techniques for the preparation of quasicrystal-forming Zr-based alloys.     

Microstructure and Mechanical Properties of Al-4.9Ni-4.9Ti Alloy Prepared by Mechanical Alloying

Mechanically alloyed Al-4.9Ni-4.9Ti powders were prepared by milling mixed aluminium, titanium and nickel powders, and then consolidated by hot hydrostatic extrusion. The microstructures of milled powders and extruded bars were characterized by X-ray diffraction and transmission eIectron microscopy observation. The results show that mechanical alloying and consolidating processes have great effects on the microstructures and mechanical properties of extruded materials. Polycrystalline materials having an ultrafine grain size may be prepared by mechanical alloying. The strength and thermal stability are improved with the increasing of processing time of mechanical alloying, since grain size decreases and volume fraction of dispersoids increases as milling time increased