Effect of temperature on solid-state formation of bulk nanograined intermetallic Al3Ni during high-pressure torsion

A bulk form of nanograined intermetallic Al₃Ni was produced by severe plastic deformation using high-pressure torsion (HPT). Powder mixtures of 75?mol% Al and 25?mol% Ni were processed by HPT at a selected temperature in the range of room temperature (RT) to 573?K under a pressure of 6?GPa. X-ray diffraction analysis revealed that the Al₃Ni intermetallic formed after processing for 50 revolutions at RT but, as the processing temperature increased, less revolutions (i.e. lower imposed strain) were required for the formation of Al₃Ni. Observations by transmission electron microscopy showed that the microstructure consists of ultrafine grains having a size of 300–2000?nm after 3 and 10 revolutions. Once the Al₃Ni formed after a higher number of revolutions, equiaxed nanograins with a size of ~30?nm prevailed with a significant increase in hardness. The increase in hardness was more significant when processed at higher temperatures because of increasing the fraction of Al₃Ni. It was shown that the solid-state formation of Al₃Ni occurred due to enhanced diffusion (i.e. decreased activation energy for diffusion) through the presence of high density of lattice defects.     

In situ electron microscopy investigations of solid-state synthesis in Al/Au thin bilayer films

In situ transmission electron microscopy investigations of solid-state synthesis in Al/Au thin bilayer films are conducted. The samples are heated in the column of a transmission electron microscope. The heating temperature is changed from room temperature to 300°C with a heating rate of up to 120°C min^?1. It is found that solid-phase synthesis starts at ≈100°C. At 140 ± 5°C, two crystal phases, Al₂Au (Fm3m) and AlAu₂ (I4/mmm), are simultaneously observed, while at 235 ± 5°C and higher (up to 300°C) only Al₂Au phase is detected.     

Solid-state synthesis in Ni/Fe/MgO(001) epitaxial thin films

Solid-state synthesis in Ni/Fe/MgO(001) bilayer epitaxial thin films has been studied experimentally. The phase sequence Fe/Ni→(～350°C)Ni₃Fe→(～400°C)NiFe→(～ 550°C)γ_par is formed as the annealing temperature increases. The crystal structure in the invar region consists of epitaxially intergrown single-crystal blocks consisting of the paramagnetic γ_par and ferromagnetic NiFe phases, which satisfy the orientation relationship [100](001)NiFe ∥ [100](001) γ_par. It has been shown that the nucleation temperatures of the Ni₃Fe, NiFe, and γ_par phases coincide with the temperatures of solid-state transformations in the Ni-Fe system.     

Solid-state synthesis and phase transformations in Ni/Fe films: Structural and magnetic studies

We have used X-ray diffraction, volume magnetocrystalline anisotropy constant and resistance measurements to study solid-state synthesis in Ni(0 0 1)/Fe(0 0 1), Ni/Fe(0 0 1) and Ni/Fe thin films with the atomic ratio between Fe and Ni of 1:1 (1Fe:1Ni), and 3:1 (3Fe:1Ni). We have found that the formation of Ni₃Fe and NiFe phases in the 1Fe:1Ni films takes place at temperatures ∼620 and ∼720 K, correspondingly. In the case of the 3Fe:1Ni films the solid-state synthesis starts with Ni₃Fe and NiFe phase formation at the same temperatures as for the 1Fe:1Ni films. The increasing of annealing temperature above 820 K leads to the nucleation of a paramagnetic γ_par phase at the FeNi/Fe interface. The final products of solid-state synthesis in the Ni(0 0 1)/Fe(0 0 1) thin films are crystallites which consist of the epitaxially intergrown NiFe and γ_par phases according to the [1 0 0](0 0 1)NiFe||[1 0 0](0 0 1)γ_par orientation relationship. The crystalline perfection and epitaxial growth of the (NiFe+γ_par) crystallites on the MgO(0 0 1) surface allow to distinguish (0 0 2)γ_par and (0 0 2)NiFe X-ray peaks (the cell parameters are: a(γ_par)=0.3600±0.0005 nm and a(NiFe)=0.3578±0.0005 nm, correspondingly). At low temperatures the paramagnetic γ_par phase undergoes the martensite _γpar→α^′${\gamma }_{\mathrm{par}}\to {\alpha }^{\prime }$ phase transition which can be hindered by thermal and epitaxial strains and epitaxial clamping with a MgO substrate. On the basis of the studies of the thin-film solid-state synthesis we predict the existence of two novel structural phase transformations at the temperatures of about 720 and 820 K for alloys of the invar region of the Fe–Ni system.     

Self-propagating high-temperature synthesis and formation of quasicrystals in Al/Mn bilayer thin films

Self-propagating high-temperature synthesis in Al/Mn bilayer thin films was investigated. It was found that a quasicrystalline phase forms after the passage of self-propagating high-temperature synthesis through the sample. It is shown that after multiple initiation (n>5) of self-propagating high-temperature synthesis in a sample the quasicrystalline phase transforms into a stable Al₆Mn phase. It is conjectured that self-propagating high-temperature synthesis can play the main role in the formation of quasicrystals in other film systems as well. Pis’ma Zh. éksp. Teor. Fiz. 68, No. 2, 121–124 (25 July 1998)     

In situ phase changes in a Fe-40 at.% Al ordered alloy during ion implantation: T.E.M. study

The radiation damage and disordering phenomena produced at room temperature during Fe⁺, Bi⁺⁺ and Xe⁺ ion implantations in a Fe-40 at.% A1 ordered alloy were studied by in situ transmission electron microscopy. Progressive, but not total disordering was achieved in the thinnest areas of the specimens during high fluence implantations (> 10¹⁵ ions/cm²). Simultaneously, the athermal formation of a new phase occurs in the case of Fe⁺ and Bi⁺⁺ implantations. The diffusion-less mechanism suggests a martensitic like transformation.

During post-implantation annealing, reordering and long-range order domain growth occurred in the temperature range up to 570 K. Above 670 K another phase appeared, which was stable up to 1070 K. The results are discussed and compared with those obtained on melt-quenched or neutron irradiated specimens of the same alloy.     

Isovector quadrupole resonance observed in the 60Ni(13C,13N)60Co reaction at E/A=100 MeV

The charge-exchange reaction 60Ni(13C,13N)60Co at E/A=100 MeV has been studied to locate isovector (deltaT=1) non-spin-flip (deltaS=0) giant resonances. Besides the giant dipole resonance at E(x)=8.7 MeV, another resonance has been observed at E(x)=20 MeV with a width of 9 MeV. Distorted-wave Born approximation analysis on the angular distribution clearly indicated the L=2 multipolarity, attributing the E(x)=20 MeV state to the giant isovector quadrupole resonance.     

Alloy formation at the Ni–Al interface for nickel films deposited on Al(110) surfaces

Alloy formation at the Ni–Al interface for thin nickel films deposited on Al(110) surfaces has been studied using high-energy ion scattering/channeling (HEIS) and X-ray photoelectron spectroscopy (XPS). For nickel atoms deposited at room temperature on Al(110), a large amount of nickel–aluminum intermixing occurs at the interface. For the first two monolayers (ML) of deposited nickel, an NiAl-like compound is formed. The intermixing continues with a different rate, forming an Ni₃Al-like compound for nickel coverages from 2 to 8 ML, at which point a nickel metal film begins to grow on the surface. Nickel atoms deposited at 250°C on the Al(110) surface exhibit no surface compound formation, but diffuse up to 400 Å into the aluminum substrate. Interatomic potentials based on the embedded-atom method (EAM) are used in a Monte Carlo approach to simulate the evolution of the Ni–Al(110) interface as a function of the nickel coverage. The calculated ion-scattering yields and X-ray photoelectron intensities from nickel and aluminum atoms in these simulated interfaces are in good quantitative agreement with the experimental results. The simulations show a high-density Ni–Al alloy forming at the Al(110) surface which apparently inhibits outward diffusion of aluminum, leading to the more nickel-rich alloy and finally nickel film growth. The ion-scattering simulations show an unusually large amount of backscattering occurring below the Ni–Al(110) interface, apparently associated with defocusing of the incident ion beam.     

Structure and phase composition of the intermetallide Ni3Al+0.5 at.% B synthesized under pressure

We have used x-ray structural analysis, together with transmission and scanning electron microscopy, to study the phase composition, structure, and elemental distribution in the intermetallide Ni₃Al+0.5 at.% B, produced by self-propagating high-temperature synthesis under pressure. It is shown that the synthesized material is an ordered alloy of the type L1₂. The phase composition of the alloy Ni₃Al+0.5 at.% B is represented by the phases Ni₃Al (the fundamental phase), grains of a layered NiAl composition, and inclusions of Ni₃B. The latter is found inside the Ni₃Al grains, in the form of surrounded particles, and at dislocations and at grain boundaries in the NiAl phase. Institute for the Physics of Strength and Materials Production. Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 9, pp. 59–64, September, 1996.     

Study of Ni/Si(1 0 0) solid-state reaction with Al addition

The characteristics of Ni/Si(1 0 0) solid-state reaction with Al addition (Ni/Al/Si(1 0 0), Ni/Al/Ni/Si(1 0 0) and Al/Ni/Si(1 0 0)) is studied. Ni and Al films were deposited on Si(1 0 0) substrate by ion beam sputtering. The solid-state reaction between metal films and Si was performed by rapid thermal annealing. The sheet resistance of the formed silicide film was measured by four-point probe method. The X-ray diffraction (XRD) was employed to detect the phases in the silicide film. The Auger electron spectroscopy was applied to reveal the element profiles in depth. The influence of Al addition on the Schottky barrier heights of the formed silicide/Si diodes was investigated by current-voltage measurements. The experimental results show that NiSi forms even with the addition of Al, although the formation temperature correspondingly changes. It is revealed that Ni silicidation is accompanied with Al diffusion in Ni film toward the film top surface and Al is the dominant diffusion species in Ni/Al system. However, no Ni_xAl_y phase is detected in the films and no significant Schottky barrier height modulation by the addition of Al is observed.     

Magnetic phase transition in Co/Cu/Ni/Cu(100) and Co/Fe/Ni/Cu(100)

Magnetic phase transitions in coupled magnetic sandwiches of Cu/Co/Cu/Ni/Cu(100) and Cu/Co/Fe/Ni/Cu(100) are investigated by photoemission electron microscopy. Element-specific magnetic domains are taken at room temperature to reveal the critical thickness at which the magnetic phase transition occurs. The results show that a coupled magnetic sandwich undergoes three types of magnetic phase transitions depending on the two ferromagnetic films' thickness. A phase diagram is constructed and explained in the process of constructing Monte Carlo simulations, which corroborate the experimental results.     

Ball milling of Fe40Ni40P20-xSix (x = 6, 10 and 14): production and characterization

Progress in the ball milling amorphization of elemental powders with the overall composition Fe₄₀Ni₄₀P_{20 ? x}Si_x (X = 6, 10 and 14) and thermally induced crystallization of obtained alloys were characterized by differential scanning calorimetry, X-ray diffraction and transmission Mössbauer spectroscopy (TMS). Diffusion of Si into Fe and Ni alloys promotes the formation of the amorphous phase, via previous formation of (Fe, Ni) phosphides. After milling for 32–64 h, most of the powders are amorphous but bcc Fe(Si) crystallites remain (about 5% in volume). TMS results indicate that homogenization of the amorphous phase occurs by interdiffusion of Ni and Fe in Fe(Si,P)-rich and Ni(Si,P)-rich zones respectively. Annealing induces structural relaxation of stresses induced by milling, growth of bcc Fe(Si) crystallites, precipitation of bcc Fe(Si) and fcc Ni–Fe, and minor phases of Ni-rich silicides and (Fe, Ni) phosphides. The main ferromagnetic phase is bcc Fe(Si) for Fe₄₀Ni₄₀P₁₀Si₁₀ powders obtained after milling for 32 h. However, it is fcc Fe–Ni for the same alloy after milling for 64 h. In the later powders, as well as for alloys with x = 6 and 14 milled for 32 h, the fcc Fe–Ni shows the Invar magnetic collapse.     

J-dependence observed in 61,62Ni (p,d) reactions at 40 MeV

The angular distributions of several l=3 transitions observed in the ^61,62Ni(p,d) reactions demonstrate a very stable j-dependence over a range of intensities and excitations energy.     

Dependence of magnetic characteristics on sputtering-power and substrate-temperature in amorphous Tb40(FeCoV)60 films

The amorphous Tb₄₀(Fe₄₉Co₄₉V₂)₆₀ films were deposited at different sputtering powers and substrate temperatures. The microstructural and magnetic characteristics were investigated by means of field emission scan electron microscope, magnetic force microscope and vibrating sample magnetometer. Our results show that with increasing sputtering power, out-of-plane coercivity decreases monotonically while saturation magnetization has a maximum value of 231 kA/m for the sample prepared at 50 W. The as-deposited alloy films are amorphous, whereas the coercivity and saturation magnetization are strongly dependent on the substrate temperature. An out-of-plane hysteresis loop with coercivity below 22 mT and saturation magnetization over 290 kA/m is obtained combining dc power and substrate temperature. The dominant mechanism of room temperature coercivity appears to be domain wall pinning, rather than nucleation under all conditions measured. The variation of saturation magnetization is similar to that of perpendicular magnetic anisotropy with either sputtering power or substrate temperature according to the difference of magnetic domain structure.     

Solid-state synthesis and atomic ordering in thin Cu/Au films (atomic ratio, Cu : Au = 3 : 1)

In situ transmission electron microscopy investigations of the processes of solid-state synthesis and atomic ordering in bilayer Cu/Au nanofilms (atomic ratio, Cu: Au = 3: 1) are conducted. It is found that solid-state synthesis starts at 170°C. A Cu₃Au atomic-disordered structure (Fm3m space group; lattice constant, a = 3.76 ± 0.01 Å) forms at 280°C. Annealing the film for 1 hour at 380°C produced a Cu₃AuI (L1₂ type) atomic-ordered superstructure, a Pm-3m space group, and lattice constant, a = 3.76 ± 0.01 Å in the bulk of the film.