Synthesis of nanocrystalline NiAl by mechanical alloying

The nanocrystalline NiAl intermetallic compound was synthesized by mechanical alloying of the elemental powders. The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometery, scanning electron microscopy and microhardness measurements. The mechanical alloying resulted in the gradual formation of nanocrystalline NiAl with a grain size of 20 nm. It was found that NiAl phase develops by continuous diffusive reaction at Ni/Al layers interfaces. The NiAl compound exhibited high microhardness value of about 1035 Hv.     

Phase evolution of Mg–Al–Zr nanophase alloys prepared by mechanical alloying

Al–Mg and Al–Mg–Zr alloys were processed by mechanical alloying. The phase constitution of the powders was strongly dependent on the composition of the starting mixture. In as-milled powders, an Al(Mg) solid solution was formed with up to 40 at% Al, which after annealing transformed to the equilibrium β-Al₃Mg₂ phase. For high Mg concentrations (60–90 at%) the dominant phase was γ-Al₁₂Mg₁₇ in accordance with the equilibrium phase diagram. The addition of Zr led to the appearance of Zr–Al intermetallics causing Mg to precipitate out of the Al(Mg) solution. The effect of zirconium was also to refine the structure and to retard grain growth.     

Characterization and formation mechanism of nanocrystalline (Fe,Ti)3Al intermetallic compound prepared by mechanical alloying

The nanocrystalline (Fe,Ti)₃Al intermetallic compound was synthesized by mechanical alloying (MA) of elemental powder with composition Fe₅₀Al₂₅Ti₂₅. The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry and microhardness measurements. Morphology and cross-sectional microstructure of powder particles were characterized by scanning electron microscopy. It was found that a Fe/Al/Ti layered structure was formed at the early stages of milling followed by the formation of Fe(Ti,Al) solid solution. This structure transformed to (Fe,Ti)₃Al intermetallic compound at longer milling times. Upon heat treatment of (Fe,Ti)₃Al phase the degree of DO₃ ordering was increased. The (Fe,Ti)₃Al compound exhibited high microhardness value of about 1050 Hv.     

X-ray diffraction study on Ni---Al---Se amorphization by mechanical alloying

In this paper, the amorphization process in mechanical alloyed Ni---Al---Se powders has been investigated by X-ray diffraction. The influence of Se on the amorphization of Ni---Al alloys, and the influence of milling time on the powder structure, microcrystallites size and phases lattice distortion are presented. Also, the Fe and Cr content from the milling medium, after 400 h, was determined.     

In situ nanocrystalline Fe–Si coating by mechanical alloying

A new approach for deposition of in situ nanocrystalline Fe–Si alloy coating on mild steel substrate by mechanical milling has been proposed. The thickness of nanocrystalline coating was a function of milling time and speed. Milling speed of 200 rpm was the optimum condition for development of uniform, hard, adherent and dense 200–300 μm thick nanocrystalline coating. A possible mechanism, consisting of three steps like repeated impact, cold welding and delamination, has been proposed for the formation of coating. These coatings have resulted in the increase of the hardness to almost double the value before coating.     

Structural and magnetic properties of nanocrystalline NiFeCuMo powders produced by wet mechanical alloying

The NiFeCuMo nanocrystalline soft magnetic powders were successfully obtained by wet mechanical alloying route in a planetary ball mill using benzene (C₆H₆) as process control agent (PCA). The milling time used was ranging from 2 up to 20 h. The synthesis conditions and alloy formation have been investigated by X-ray and neutron diffraction as well as their influence on the intrinsic physical properties. Nanometer scale (≈10 nm) crystallites were obtained. A decrease of the samples magnetization has been observed and attributed to the stresses induced during the milling and to the benzene adsorbed on the powders surface. Differential scanning calorimetry investigation shows the presence of an exothermic peak related to the presence of benzene. The adsorbed benzene, internal stresses and crystalline defects removal took place during the heat treatment at 350 °C for 4 h, leading to an improvement of the powders magnetization.     

Nanophase intermetallic FeAl obtained by sintering after mechanical alloying

The preparation of bulk nanophase materials from nanocrystalline powders has been carried out by the application of sintering at high pressure. Fe–50 at.%Al system has been prepared by mechanical alloying for different milling periods from 1 to 50 h, using vials and balls of stainless steel and a ball-to-powder weight ratio (BPR) of 8:1 in a SPEX 8000 mill. Sintering of the 5 and 50 h milled powders was performed under high uniaxial pressure at 700 °C. The characterization of powders from each interval of milling was performed by X-ray diffraction, Mössbauer spectroscopy, scanning and transmission electron microscopy. After 5 h of milling formation of a nanocrystalline α-Fe(Al) solid solution that remains stable up to 50 h occurs. The grain size decreases to 7 nm after 50 h of milling. The sintering of the milled powders resulted in a nanophase-ordered FeAl alloys with a grain size of 16 nm. Grain growth during sintering was very small due to the effect of the high pressure applied.     

Application of controlled and electrical discharge assisted mechanical alloying for the synthesis of nanocrystalline MgB2 superconducting compound

In this paper we present the results of our efforts to synthesize the nanocrystalline MgB₂ superconducting compound from elemental Mg and B powders by combination of controlled mechanical pre-alloying in a magneto-mill Uni-Ball-Mill 5 under shearing mode followed by electrical discharge (ED) assisted mechanical alloying (MA). There is no conclusive evidence of MgB₂ formation in the Mg-2B mixture using crystalline boron after controlled mechanical alloying (CMA) under protective argon or helium atmosphere as well as subsequent ED assisted alloying. There seems to be some XRD evidence of the strongest (1 0 1) MgB₂ peak presence in the Mg-2B mixture processed using both crystalline and amorphous boron after CMA under hydrogen as well as subsequent ED assisted alloying but this evidence is rather ambiguous. We postulate here that it is highly likely that a certain critical Mg nanograin size must be achieved before a successful reaction to form nanocrystalline MgB₂ is going to be completed. Following recent report by Gümbel et al. [Appl. Phys. Lett. 80 (2002) 2725] this critical value can be roughly estimated at 15 nm or less. Calculations of the Mg nanograin size in the present work show that only three Mg-2B powders ball milled under hydrogen meet this critical nanograin size criterion for the Mg phase. However, a massive formation of the β-MgH₂ hydride in these powders consumes the available Mg in the reaction with hydrogen which may leave inadequate concentration of Mg to form MgB₂ even though the nanograin size of Mg is sufficiently refined, say below 15 nm.     

Development of nano-structure Cu-Zr alloys by the mechanical alloying process

Cu-Zr alloys have many applications in electrical and welding industries for their high strength and high electrical and thermal conductivities. These alloys are among age-hardenable alloys with capability of having nano-structure with high solute contents obtainable by the mechanical alloying process. In the present work, Cu-Zr alloys have been developed by the mechanical alloying process. Pure copper powders with different amounts of 1, 3 and 6 wt% of commercial pure zirconium powders were mixed. The powder mixtures were milled in a planetary ball mill for different milling times of 4, 12, 48 and 96 h. Ball mill velocity was 250 rpm and ball to powder weight ratio was 10:1. Ethanol was used as process control agent (PCA). The milling atmosphere was protected by argon gas to prevent the oxidation of powders. The milled powders were analysed by XRD technique and were also investigated by SEM observations. Lattice parameters, crystal sizes and internal strains were calculated using XRD data and Williamson-Hall equation. Results showed that the lattice parameter of copper increased with increasing milling time. The microstructure of milled powder particles became finer at longer milling time towards nano-scale structure. SEM observations showed that powder particles took plate-like shapes. Their average size increased initially and reached a maximum value then it decreased at longer milling times. Different zirconium contents had interesting effects on the behavior of powder mixtures during milling.     

Preparation of W–Al–Mo ternary alloys by mechanical alloying

Single phase W_XAl₅₀Mo_50−X (X = 40, 30, 20 and 10) powders have been synthesized directly by mechanical alloying (MA). The structural evolutions during MA and subsequent as-milled powders by annealing at 1400 °C have been analyzed using X-ray diffraction (XRD). Different from the Mo₅₀Al₅₀ alloy, W₄₀Al₅₀Mo₁₀ and W₃₀Al₅₀Mo₂₀ alloys were stable at 1400 °C under vacuum. The results of high-pressure sintering indicated that the microhardnesses of two compositions, namely W₄₀Al₅₀Mo₁₀ and W₃₀Al₅₀Mo₂₀ alloys have higher values compared with W₅₀Al₅₀ alloy.     

Structural, microstructural and magnetic properties of amorphous/nanocrystalline Ni63Fe13Mo4Nb20 powders prepared by mechanical alloying

This paper focuses on the magnetic, structural and microstructural studies of amorphous/nanocrystalline Ni₆₃Fe₁₃Mo₄Nb₂₀ powders prepared by mechanical alloying. The ball-milling of Ni, Fe, Mo and Nb powders leads to alloying the element powders, the nanocrystalline and an amorphization matrix with Mo element up to 120 h followed by the strain and thermal-induced nucleation of a single nanocrystalline Ni-based phase from the amorphous matrix at 190 h. The results showed that the saturation magnetization decreases as a result of the electronic interactions between magnetic and non-magnetic elements and finally increases by the partial crystallization of the amorphous matrix. The coercive force increases as the milling time increases and finally decreases due to sub-grains formation.     

Direct synthesis of MgCNi3 by mechanical alloying

MgCNi₃, an intermetallic compound with superconductivity, was synthesized from the Mg (or Mg₂Ni), Ni and graphite powders by mechanical alloying (MA). It is shown that the preliminary condition for the formation of MgCNi₃ is that Mg₂Ni must form in advance of MgCNi₃ in the MA process or be the starting component.     

Phase formation during mechanical alloying and subsequent low-temperature heat treatment of Al–27.4at%Fe–28.7at%C powders

Phase formation during high energy ball milling of a ternary elemental powder mixture with a composition of Al–27.4at%Fe–28.7at%C and during low temperature heat treatment of the milled powder was studied. It was found that an amorphous phase formed during prolonged milling. During heating the shorter time milled powder, Al and Fe reacted first, forming the AlFe phase and then at a higher temperature, AlFe reacts with Fe and C, forming the AlFe₃C_0.5 phase. During heating the longer time milled powder which contains a substantial amount of amorphous phase, the amorphous phase partially crystallizes first, forming the AlFe and AlFe₃C_0.5 phases, and then AlFe reacts with the remaining amorphous phase, forming the AlFe₃C_0.5 phase. Overall, mechanical alloying of Al, Fe and C elemental phases enables formation of an amorphous phase, while low temperature heat treatment of mechanically milled powder facilitates formation of AlFe and AlFe₃C_0.5 phases.     

Microstructural characterization and amorphous phase formation in Co40Fe22Ta8B30 powders produced by mechanical alloying

In this work, microstructural evolution and amorphous phase formation in Co₄₀Fe₂₂Ta₈B₃₀ alloy produced by mechanical alloying (MA) of the elemental powder mixture under argon gas atmosphere was investigated. Milling time had a profound effect on the phase transformation, microstructure, morphological evolution and thermal behavior of the powders. These effects were studied by the X-ray powder diffraction (XRD) in reflection mode using Cu Kα and in transmission configuration using synchrotron radiation, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The results showed that at the early stage of the milling, microstructure consisted of nanocrystalline bcc-(Fe, Co) phases and unreacted tantalum.Further milling, produced an amorphous phase, which became a dominant phase with a fraction of 96 wt% after 200 h milling. The DSC profile of 200 h milled powders demonstrated a huge and broad exothermic hump due to the structural relaxation, followed by a single exothermic peak, indicating the crystallization of the amorphous phase. Further XRD studies in transmission mode by synchrotron radiation revealed that the crystalline products were (Co, Fe)_20.82Ta_2.18B₆, (Co, Fe)₂₁ Ta₂ B₆, and (Co, Fe)₃B₂. The amorphization mechanisms were discussed in terms of severe grain refinement, atomic size effect, the concept of local topological instability and the heat of mixing of the reactants.     

Microstructure evolution and mechanical properties of nanocrystalline FeAl obtained by mechanical alloying and cold consolidation

In the present study high energy mechanical milling followed by cold temperature pressing consolidation has been used to obtain bulk nanocrystalline FeAl alloy. Fully dense disks with homogenous microstructure were obtained and bulk material show grain size of 40 nm. Thermal stability of the bulk material is studied by XRD and DSC techniques. Subsequent annealing at a temperature up to 480 °C for 2 h of the consolidated samples enabled supersaturated Fe(Al) solid solution to precipitate out fine metastable Al₅Fe₂, Al₁₃Fe₄ and Fe₃Al intermetallic phases. Low temperature annealing is responsible for the relaxation of the disordered structure by removing defects initially introduced by severe plastic deformation. Microhardness shows an increase with grain size reduction, as expected from Hall-Petch relationship at least down to a grain size of 74 nm, then a decrease at smallest grain sizes. This could be an indication of some softening for finest nanocrystallites. The peak hardening for the bulk nanocrystalline FeAl is detected after isochronal ageing at 480 °C.     

Microstructure evolution in nanocrystalline Cu-Nb alloy during mechanical alloying

The microstructural evolution of nanocrystalline Cu-10%Nb（mass fraction） alloy during mechanical alloying （MA） was investigated by using X-ray diffraction, optical microscopy（OM）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM） observation. Upon milling of Cu-Nb powders with coarse grains, the grain size is found to decrease gradually with lengthening milling time, and reach the minimum value （about 9 nm） after 100 h milling. The microstrain and the microhardness of the powders increase during the grain refinement. And Cu lattice parameter increases steadily over 100 h milling. The mechanisms of solid solution extension during milling were discussed. The results show that up to 10%Nb can be brought into solid solution by MA. The extension of solid solution is found to relate closely with the formation of nanocrystalline.     

Phase transformation of the CuAl2 intermetallic alloy during high-energy ball-milling

In the present investigation, we have studied the phase transformation of the CuAl₂ intermetallic alloy with tetragonal structure by high-energy ball-milling. The structural changes with milling time were followed by X-ray diffraction, differential scanning calorimetry and electron microscopy. It is found that CuAl₂-phase transforms to body centered cubic structure after a long periods of high-energy ball-milling time. According to SEM results, the milling powders change their mechanical behavior from brittle to ductile during the phase transformation. Rietveld analysis showed that around 29% of unit cells in the metastable cubic structure are occupied by Cu suggesting Al segregation in the material and explaining the change in the mechanical behavior of the alloy.     

PAS consolidating behavior of mechanically alloyed nanocrystalline NiAl intermetallic compound

In this study, nanocrystalline NiAl intermetallic compound was obtained by mechanical alloying and PAS (plasma activated sintering method). Nanocrystalline NiAl powder was fabricated after 30 hr of milling with 2 wt.% stearic acid added as a PCA (process control agent) to the Ni-50at%Al composition. The grain size of the nanocrystalline NiAl powder was about 10 nm. Nanocrystalline NiAl powder was consolidated at 1000°C, 1100°C, 1200°C and 1300°C for 2 min with 30 MPa compressive force. The surface morphology of the NiAl consolidated at 1300°C was very regular and dense, above 96% of theoretical density (5.9 g/cm³). Al₄C₃ was observed in the NiAl consolidated at 1300°C by TEM analysis. It is thought that the carbons came from the stearic acid during the MA process and the graphite mold during the PAS process. The grain size of the NiAl consolidated at 1300°C did not increase but the grain shape became flat due to compressive force.     

Synthesis and characterization of nanocrystalline AlFeTiCrZnCu high entropy solid solution by mechanical alloying

Traditional alloys are based on one or two major alloying elements. High entropy alloys are equiatomic multicomponent alloys, wherein configurational entropy is maximized to obtain single phase solid solutions. The present paper reports synthesis of nanostructured equiatomic high entropy solid solutions from binary to hexanary compositions in Al–Fe–Ti–Cr–Zn–Cu system by mechanical alloying. These alloys have BCC structure with crystallite size less than 10 nm. The high entropy solid solution in these alloys is stable even after annealing at 800 °C for 1 h. The hardness of AlFeTiCrZnCu solid solution is 2 GPa in the sintered condition with a density of 99%. The similar nanostructured solid solutions have also been synthesized in CuNiCoZnAlTi and NiFeCrCoMnW alloys.     

Microstructural and mechanical properties of Al-Mg/Al2O3 nanocomposite prepared by mechanical alloying

The effect of milling time on the microstructure and mechanical properties of Al and Al-10 wt.% Mg matrix nanocomposites reinforced with 5 wt.% Al₂O₃ during mechanical alloying was investigated. Steady-state situation was occurred in Al-10Mg/5Al₂O₃ nanocomposite after 20 h, due to solution of Mg into Al matrix, while the situation was not observed in Al/5Al₂O₃ nanocomposite at the same time. For the binary Al-Mg matrix, after 10 h, the predominant phase was an Al-Mg solid solution with an average crystallite size 34 nm. Up to 10 h, the lattice strain increased to about 0.4 and 0.66% for Al and Al-Mg matrix, respectively. The increasing of lattice parameter due to dissolution of Mg atom into Al lattice during milling was significant. By milling for 10 h the dramatic increase in microhardness (155 HV) for Al-Mg matrix nanocomposite was caused by grain refinement and solid solution formation. From 10 to 20 h, slower rate of increasing in microhardness may be attributed to the completion of alloying process, and dynamic and static recovery of powders.