Structure and phase transformations in Fe–Ni–Mn alloys nanostructured by mechanical alloying

Ternary Fe₈₆Ni_xMn_14−x alloys, where x = 0, 2, 4, 6, 8, 10, 12, 14, 16 at.%, were prepared by the mechanical alloying (MA) of elemental powders in a high-energy planetary ball mill. X-ray diffraction analysis and Mössbauer spectroscopy were used to investigate the structure and phase composition of samples. Thermo-magnetic measurements were used to study the phase transformation temperatures. The MA results in the formation of bcc α-Fe and fcc γ-Fe based solid solutions, the hcp phase was not observed after MA. As-milled alloys were annealed with further cooling to ambient or liquid nitrogen temperatures. A significant decrease in martensitic points for the MA alloys was observed that was attributed to the nanocrystalline structure formation.     

Structure, hyperfine interactions and magnetization studies of mechanically alloyed Fe50Ge50 and Fe62Ge38

X-ray diffraction, Mössbauer spectroscopy and magnetization measurements were used to study the structure and some magnetic properties of Fe₅₀Ge₅₀ and Fe₆₂Ge₃₈ prepared by mechanical alloying from the elemental powders. In both cases in the early stages of milling the intermediate paramagnetic FeGe₂ phase was formed. The mechanical alloying process of Fe₅₀Ge₅₀ resulted in the formation of the paramagnetic FeGe (B20) phase with an average crystallite size of about 15 nm. In the case of the Fe₆₂Ge₃₈, the ferromagnetic Fe₅Ge₃ (β) phase with a Curie temperature of about 430 K was obtained. The average crystallite size was about 9 nm. The average hyperfine magnetic field of about 16 T allowed it to determine that more than four germanium atoms exist in the nearest environment of the ⁵⁷Fe isotopes in the Fe₅Ge₃ phase.     

Magnetic and structural studies of mechanically alloyed (Fe50Co50)62Nb8B30 powder mixtures

Amorphous (Fe₅₀Co₅₀)₆₂Nb₈B₃₀ powder mixture was prepared by mechanical alloying from elemental Fe, Co, B and Nb powders in a planetary ball mill under argon atmosphere. Structural, thermal and magnetic properties were performed on the milled powders by means of X-ray diffraction, differential scanning calorimetry and magnetic measurements. The amorphous state is reached after 125 h of milling. The excess enthalpy due to the high density of defects is released at temperature below 300 °C. Crystallisation and growth of crystal domains are the dominating processes at high temperatures. The saturation magnetisation decreases rapidly during the first 25 h of milling to about 15.24 A m²/kg and remains nearly constant on further milling. Coercivity, H_c, value of about 160 Oe is obtained after 125 h of milling.     

On the general outline of physical properties of amorphous-nanocrystalline Fe-Cr-Mn-N alloy powders prepared by mechanical alloying under nitrogen

This paper reviews last findings about physical properties of Fe-Cr-Mn-N powders synthesized by mechanical alloying under nitrogen. Their thermal, magnetic, indentation, and grain growth behaviors and nitrogen distribution in their amorphous-nanocrystalline structure are regarded as a function of milling time. Particularly, the role of nitrogen in the aforementioned phenomena is reviewed in detail.     

Milling and subsequent thermal annealing effects on the microstructural and magnetic properties of nanostructured Fe90Co10 and Fe65Co35 powders

The influence of milling and subsequent annealing on the microstructural and magnetic properties of Fe₉₀Co₁₀ and Fe₆₅Co₃₅ alloys is investigated. After milling for 8 h a body-centred cubic nanostructured Fe–Co alloy forms with an average crystallite size of about 12 nm. The magnetization saturation (M_S) increases 16% for Fe₆₅Co₃₅ and 5% for Fe₉₀Co₁₀ alloys by milling for 8 h. Subsequent annealing of Fe₉₀Co₁₀ and Fe₆₅Co₃₅ powders for 105 min at 550 °C improves the M_S about 6 and 11%, respectively. Before annealing, the coercivity increases (up to 60 Oe) by milling for 3 h, followed by a reduction on milling for longer periods (45 h). At the initial stage of the heating, a sharp decrease in H_C to 8–10 Oe occurs due to the relief of internal strain. Further heating leads to an increase in the coercivity (intermediate times) followed by a slight diminution on heating for final stage.     

The synthesis of nanocrystalline Ni75Nb12B13 alloys by high energy ball milling of elemental components

Ni₇₅Nb₁₂B₁₃ alloys were synthesized by mechanical alloying (MA) of individual Ni, Nb and B components. X-ray investigation showed the formation of Ni (Nb, B) solid solution and amorphous phase at the intermediate stage of milling. Metastable phases formed by MA turned into Ni (Nb), Ni₂₁Nb₂B₆ and Ni₃Nb stable phases during heating up to 720 °C. The exothermal effects on DSC curves were caused with these processes. The disintegration of Ni (Nb, B) solid solution and crystallization of an amorphous phase resulted in the stable phases formation during the milling prolongation as well as after thermal treatment.     

Synthesis and characterization of mechanical-alloyed Ti–xMg alloys

The synthesis and characterization of Ti–xMg (x=4, 9, 12, 15, 21, 24 at%) alloys using mechanical alloying was investigated. A nanometer-sized Ti–24Mg alloy was produced. During mechanical alloying, the height of the XRD peaks of the Mg in the Ti–9Mg alloy decreased, and then disappeared, whereas the Ti XRD peaks broadened, and the grain size decreased with increasing milling time. The Mg firstly dissolved in the grain boundaries of the Ti, and then diffused into the Ti grain interiors. The grain boundaries played an important role in enhancing the solid solubility of Mg in Ti. With increasing Mg content the volume fraction of grain boundaries increased, and a decrease in grain size occurred after mechanical alloying for 48 h.     

Nanocrystalline spherical iron–nickel (Fe–Ni) alloy particles prepared by ultrasonic spray pyrolysis and hydrogen reduction (USP-HR)

FeCl₂ and NiCl₂ were used for synthesis of nanocrystalline spherical Fe–Ni alloy particles by ultrasonic spray pyrolysis and hydrogen reduction (USP-HR). Spherical ultrafine Fe–Ni particles were obtained by USP of aqueous solutions of iron–nickel chloride followed by thermal decomposition of generated aerosols in hydrogen atmosphere. Particle sizes of the produced Fe–Ni particles can be controlled by the change of the concentration of an initial solution. The effect of the precursor solution in the range of 0.05, 0.1, 0.2 and 0.4 M on the morphology and crystallite size of the Fe–Ni alloy particles are investigated under the conditions of 1.5 h running time, 900 °C reduction temperature, and 1.0 L/min H₂ volumetric flow rate. X-ray diffraction (XRD) studies and Scherrer crystallite size calculations show that the crystalline size was nearly 28 nm. Energy dispersive spectroscopy (EDS) was performed to determine the chemical composition of the particles. Transmission electron microscope (TEM) was used to confirm the crystalline size, that was determined using XRD results. Scanning electron microscopy (SEM) observations reveal that the precursor solution strongly influences the particle size of the synthesized Fe–Ni alloy particles. Spherical nanocrystalline Fe–Ni alloy particles in the range of 80 and 878 nm were obtained at 900 °C.     

Glass-forming ability and magnetic properties of mechanically solid-state reacted Co100−xTix alloy powders

A high-energy ball milling technique using the mechanical alloying method has been employed for fabrication of glassy Co_100−xTi_x (25≤x≤67) alloy powders at room temperature. The fabricated glassy alloys in the Co-rich (33≥x) side exhibit good soft magnetic properties. The binary glassy alloys for which the glass transition temperatures (T_g) have rather high temperatures (above 800 K), show large supercooled liquid regions before crystallization (ΔT_x larger than 50 K). The reduced glass transition temperature (ratio between T_g and liquidus temperatures, T_l (T_g/T_l)) was found to be larger than 0.56. We have also performed post-annealing experiments on the mechanically deformed Co/Ti multilayered composite powders. The results show that annealing of the powders at 710 K leads to the formation of a glassy phase (thermally enhanced glass formation reaction), of which the heat of formation was measured directly. The similarity in the crystallization and magnetization behaviors between the two classes of as-annealed and as-mechanically alloyed glassy powders implies the formation of the same glass state.     

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.     

Quantitative analysis of phases formed in the aluminothermic reduction of Ta2O5 by plasma

A novel technique of aluminothermic reduction of tantalum oxide is developed to produce tantalum in form of powder. In this technique, hydrogen plasma is used to trigger the reaction in a plasma reactor. The reacted powders were analyzed by XRD and SEM. Rietveld method was used to quantify the phases present in the product of reaction. The results showed that a tantalum rich phase with a dendritic structure, typical of molten phases is formed. This phase occurred in significant amounts onto the surface and in bulk of the reacted grains.     

Formation of Al–Y oxide during processing of γ-TiAl

While processing Y₂O₃ dispersed γ-TiAl, Y₂O₃ particles which dissolved during hot isostatic pressing (HIP’ing) were found to precipitate during the heat treatment in the form of a mixed Al–Y oxide. To understand the chemical reaction that occurs between Y₂O₃ and γ-TiAl during the heat treatment cycle, a powder mixture comprising of γ-TiAl and 10 wt.% Y₂O₃ was mechanically alloyed (MA’d) for 8 h and the milled powder was subjected to differential thermal analysis (DTA) at 1150 °C prior to analyzing it using X-ray diffraction technique. The present study clearly demonstrates that aluminum in the combined form either as γ-TiAl or Al₂O₃ reacts in a similar manner with Y₂O₃ when milled and heat treated at 1150 °C. In either case there is formation of Al₂Y₄O₉ (2Y₂O₃.Al₂O₃).     

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.     

Electrochemical syntheses of soft and hard magnetic Fe50Pd50-based nanotubes and their magnetic characterization

Near-equiatomic Fe-Pd-based nanotubes with diameters of 200 nm and lengths of 1 μm were directly electrodeposited from a single electrolyte into polycarbonate templates. The as-deposited Fe₅₀Pd₅₀ nanotubes were then characterized compositionally, structurally and magnetically. The as-deposited Fe₅₀Pd₅₀ tubes had an fcc crystal structure and were magnetically soft (H_C ≈ 10 kA/m), with the easy axis of the magnetization being parallel to the axes of the tubes. Angular-dependence measurements of the coercivity, where the hysteresis loops were measured as a function of the angle (θ) of the applied demagnetizing field, revealed a combination of magnetization reversal mechanisms, consisting of the curling mechanism, which dominates at low angles, with a transition to coherent rotation at angles ≥70°. The development of the coercivity with annealing temperature due to the L1₀ ordering was also investigated. For this purpose the as-deposited nanotubes were annealed at temperatures from 400 °C to 650 °C for 1 h in Ar + 7% H₂ and the phase formation, the microstructure and the magnetic properties were analyzed. A maximum in the coercivity of 135 kA/m was achieved upon annealing at 550 °C.     

Mechanochemical solid state synthesis of (Cd0.8Zn0.2)S quantum dots: Microstructure and optical characterizations

(Cd_0.8Zn_0.2)S quantum dots with a mixture of both cubic (Zinc-blende) and hexagonal (Wurtzite) phases have been prepared within 75 min by mechanical alloying the stoichiometric mixture of Cd, Zn and S powders at room temperature in a planetary ball mill under Ar. The Rietveld analysis of X-ray powder diffraction data reveals relative phase abundances of both cubic and hexagonal phases and several microstructure parameters like lattice parameters, particle sizes, lattice strains, concentrations of different kinds of stacking faults, etc. in both the phases. At the time of formation, hexagonal phase dominates over the cubic phase (molar ratio ∼0.6:0.4), but in course of milling up to 15 h, the hexagonal phase partially transforms to cubic phase and the molar ratio becomes ∼0.4:0.6. Particle sizes of hexagonal and cubic phases reduce to ∼4.5 nm and 12.5 nm, respectively, after 15 h of milling. The hexagonal phase contains a significant amount of lattice strain in comparison to cubic phase. The presence of different kinds of stacking faults is revealed clearly from the high resolution transmission electron microscope (HRTEM) images.