Microstructural investigation of Fe–Zr–B–Ag soft magnetic thin films

A microstructural study of DC-sputtered Fe_93−xZr₃B₄Ag_x films on Si(0 0 1) substrates has been carried out using X-ray diffraction (XRD) and transmission electron microscopy (TEM). All samples were deposited as a function of additive Ag content (x=0–6 at%), and annealed in the range of temperature, 300–600°C, for 1 h in order to obtain enhanced soft magnetic properties. Through XRD and TEM investigation, Ag-free Fe₉₃Zr₃B₄ films on Si(0 0 1) substrates consisted of nano-crystalline Fe-based phases. In the presence of Ag additive element, the microstructure of as-deposited Fe_93−xZr₃B₄Ag_x films consisted of a mixture of majority of Fe-based amorphous and Ag crystalline phases. In this case, additive element, Ag played a role in retarding the formation of Fe-based crystalline phases during deposition, and insoluble nano-crystalline Ag particles were dispersed in the Fe-based amorphous matrix. As the content of Ag increased, the intensity of Ag crystalline XRD peak increased. Crystallization of Fe-based amorphous phase in the matrix of Fe₈₈Zr₃B₄Ag₅ thin films occurred at an annealing temperature of 400°C. In the case of Fe₈₈Zr₃B₄Ag₅ films annealed at 500°C, a much enhanced permeability of the Fe-based alloy thin films associated with nano-crystalline phases was achieved.     

Structure and magnetic properties of co-sputtered Co–C thin films

We studied the structure and magnetic properties of co-sputtered Co_1−xC_x thin films using a transmission electron microscope (TEM) and a SQUID magnetometer. These properties were found to depend critically on deposition temperature, T_S, and composition, x. Generally, phase separation into metallic Co and graphite-like carbon phases proceeds with increasing T_S and decreasing x. Plan view and cross-sectional TEM images of the films prepared showed that Co grains about 10–20 nm in diameter and 30–50 nm in height are three-dimensionally separated by graphite-like carbon layers 1–2 nm thick. Optimum magnetic properties with saturation magnetization of 380 emu/cc and coercivity of 400 Oe were obtained for a film with x=0.5 and T_S=350°C.     

Study of nanocrystalline Fe－Al－N soft magnetic thin films

Fe－Al－N films were fabricated by reactive sputtering using a radio-frequency magnetron sputtering system. The effects of Al and N content and annealing temperature on microstructure and magnetic properties were investigated. The Fe－Al－N films, which have good soft magnetic properties, consist of nanocrystalline α-Fe grains and a small amount of other phases in the boundaries of α-Fe grains. The average α-Fe grain size is about 10－15nm. A slight amount of Fe－N and Al－N compounds precipitate in the boundaries of α-Fe grains and suppress their growth. Annealing improves the soft magnetic properties slightly by releasing the residual stress and reducing defects.     

The high frequency magnetic properties of self assembled Fe–Co–Si–N nanogranular thin films

The effect of a variation in Si and N concentration on the microstructure, crystal structure and high-frequency magnetic properties of Fe–Co–Si–N nanogranular thin films was investigated. The films, prepared by rf magnetron sputtering, consisted of nanosized grains of FeCo as well as a Si and N rich intergranular amorphous phase. The Si concentration had a significant effect on the crystal structure of the FeCo phase. The resistivities of the Fe–Co–Si–N films were significantly enhanced by an increase in Si concentration. The resonant frequency of the Fe–Co–Si–N films could be tuned from 0.45 GHz to 2.1 GHz by controlling Si concentration. The N concentration greatly influenced magnetic properties and the variation in resonant frequency is in agreement with Kittel’s equation.     

Structural and magnetic properties of Si1−xGex thin films implanted with Fe ions

A series of Si_1?xGe_x (x = 1, 0.848, 0.591, 0.382, 0.209, 0.064, 0) thin films prepared by ion beam sputtering were implanted with Fe ions to different doses using the metal vapor vacuum arc technique. X-ray absorption fine structure (XAFS) was used to characterize the local microstructure around the Fe atoms in Fe-doped Si_1?xGe_x samples. Structural analysis showed that for annealed samples of Ge-rich thin films (including pure Ge) implanted with low doses of Fe ions, almost all the Fe ions substituted at Ge sites. However, an anti-ferromagnetic Fe₆Ge₅ impurity phase existed in the annealed samples implanted with high doses of Fe. It was also found that the solubility of Fe ions was highest in pure Ge films and that with increasing Si concentration, the solubility decreased. Magnetic analysis showed that for the as-implanted and annealed samples of Ge-rich thin films implanted with Fe ions, room-temperature ferromagnetism was strongest in the pure Ge series of samples and that as the Ge concentration decreased, the ferromagnetism at room temperature weakened. In addition, annealing could increase the number of Fe ions at substitution sites, which resulted in the observed increase in the saturated magnetization after annealing. Experiment and theoretical analysis showed that the ferromagnetism of Fe-doped Ge-rich Si_1?xGe_x thin films samples originated from the s, p–d exchange interactions between the Si_1?xGe_x matrix and those Fe ions which substituted at Ge sites and that the ferromagnetism was mediated by carriers.     

Role of electrolyte pH on structural and magnetic properties of Co–Fe films

Co–Fe films were electrodeposited on polycrystalline Titanium substrates from the electrolytes with different pH levels. X-ray diffraction (XRD) was used to study the crystal structure of the films. The XRD patterns showed that the films grown at the pH levels of 3.70 and 3.30 have a mixed phase consisting of face-centred cubic (fcc) and body-centred cubic, while those grown at pH=2.90 have only fcc structure. It was observed that the film composition, by energy dispersive x-ray spectroscopy, contain around 88 at% Co and 12 at% Fe for all films investigated in this study. Morphological observations indicated that all films have grainy structure with the slight change of grain size depending on the electrolyte pH. Magnetoresistance measurements, made at room temperature, showed that all films exhibited anisotropic magnetoresistance, which is affected by the electrolyte pH. From the magnetic measurements made by vibrating sample magnetometer, the saturation magnetization increases as the electrolyte pH decreases. Furthermore, all films have in-plane easy-axis direction of magnetization.     

Microstructures and soft magnetic properties of Fe80P20-xSix (x = 4.5–6.5) amorphous ribbons

Fe-based amorphous ribbons with excellent soft magnetic properties and mechanical properties were prepared in the Fe–Si–P ternary system. Enhanced soft magnetic properties could be achieved through annealing treatment of the ribbons for 1 h at 325 °C, which is far below the glass transition temperatures (462–474 °C). Icosahedral medium-range ordering with a size range of around 2 nm occurred throughout the amorphous matrix during the low-temperature annealing treatment. The annealed ribbons exhibited improved magnetic saturation of over 185 emu/g while maintaining good mechanical flexibility. During icosahedral ordering, the distance between the Fe atoms and the coordination number within the amorphous ribbon can be optimised for achieving high magnetic saturation. However, nanocrystallisation of the SiP and Fe₂P transition phases embedded within the amorphous matrix occurred after the annealing treatment for 1 h at 385 °C, which caused deterioration of the soft magnetic properties and mechanical flexibility of the ribbons. Therefore, the combination of high magnetic saturation and mechanical flexibility of the amorphous ribbons could be optimised through low-temperature annealing treatment without any nanocrystallisation.     

The microstructure and magnetic properties of electrodeposited Co–Pt thin films on Ru buffer layer

For high-density magnetic recording media, this study examined the crystal structure and the texture of electrodeposited cobalt–platinum (Co–Pt) films on Ru buffer layer. A 15-nm-thick Co–Pt film exhibited very high out-of-plane coercivity and squareness, which were 6248 Oe and 0.89, respectively. The coercivity, H_c, of Co–Pt films grown on Ru buffer layer decreased significantly with increasing thickness, possibly due to the lattice misfit of 5.4% between Co–Pt and Ru, leading to the decrease of perpendicular magnetic anisotropy (PMA) of Co–Pt films as indicated by the observed hexagonal-closed-packed (HCP) (1 1¯ 0 1) plane of Co–Pt films. According to nano beam diffraction pattern (NBDP), however, Co–Pt film grown on Ru layer of HCP exhibited mixed HCP and FCC phases. Also, cross-sectional TEM image suggests that the high PMA may result from the columnar structure of physically isolated Co–Pt grains with the c-axis perpendicular to the film plane.     

Electrical and optical properties of a-SexTe100–x thin films

The dc electrical conductivity of as deposited thin films of a-Se_xTe_100?x (x=3, 6, 9 and 12) is measured as a function of temperature range from 298 to 383 K. It is observed that the dc conductivity increases exponentially with the increase in temperature in this glassy system. The value of activation energy calculated from the slope of ln σ_dc vs. 1000/T plot, is found to decrease on incorporation of dopant (Se) content in the Te system. On the basis of pre-exponetial factor (σ₀), it is suggested that the conduction is due to thermally assisted tunneling of the carriers in the localized states near the band edges. The optical absorption measurements show an indirect optical band gap in this system and it decreases on increasing Se concentration. The optical constants (extinction coefficient (k) and refractive index (n)) do change significantly with the photon energy and also with the dopant Se concentration. The decrease in optical band gap may be due to the decrease in activation energy in the present system. It is also found that the real and imaginary parts of dielectric constants show a significant change with the photon energy as well as with the dopant concentration. With large absorption coefficients and compositional dependence of optical band gap and optical constants (n and k), these materials may be suitable for optical disk applications.     

Structural and magnetic properties of Fe–Ni mecanosynthesized alloys

Fe_100???x Ni _x samples with x?=?22.5, 30.0 and 40.0 at.% Ni were prepared by mechanical alloying (MA) with milling times of 10, 24, 48 and 72 h, a ball mass to powder mass (BM/PM) ratio of 20:1 and rotation velocity of 280 rev/min. Then the samples were sintered at 1,000°C and characterized by X-ray diffraction (XRD) and transmission Mössbauer spectrometry (TMS). From the refinement of the X ray patterns we found in this composition range two crystalline phases, one body centered cubic (BCC), one face centered cubic (FCC) and some samples show FeO and Fe₃O₄ phases. The obtained grain size of the samples shows their nanostructured character. Mössbauer spectra were fitted using a model with two hyperfine magnetic field distributions (HMFDs), and a narrow singlet. One hyperfine field distribution corresponds to the ferromagnetic BCC grains, the other to the ferromagnetic FCC grains (Taenite), and the narrow singlet to the paramagnetic FCC grains (antitaenite). Some samples shows a paramagnetic doublet which corresponds to FeO and two sextets corresponding to the ferrimagnetic Fe₃O₄ phase. In this fit model we used a texture correction in order to take into account the interaction between the particles with flake shape and the Mössbauer $\upgamma$ -rays.     

Effect of oxygen partial pressure on the structure and properties of Cu–Al–O thin films

We have studied the electrical and optical properties of Cu–Al–O films deposited on silicon and quartz substrates by using radio frequency (RF) magnetron sputtering method under varied oxygen partial pressure P_O. The results indicate that P_O plays a critical role in the final phase constitution and microstructure of the films, and thus affects the electrical resistivity and optical transmittance significantly. The electrical resistivity increases with the increase of P_O from 2.4 × 10^?4 mbar to 7.5 × 10^?4 mbar and afterwards it decreases with further increasing P_O up to 1.7 × 10^?3 mbar. The optical transmittance in visible region increases with the increase of P_O and obtains the maximum of 65% when P_O is 1.7 × 10^?3 mbar. The corresponding direct band gap is 3.45 eV.     

Preparation and magnetic properties of Fe–Ag granular alloy

An aqueous solution of AgNO₃ in the presence of ammonia and Fe(CO)₅ is sonicated under a H₂/Ar mixture, yielding a nanostructured homogeneous phase of Ag/Fe₂O₃. This composite material is further reduced at 300°C under hydrogen to produce the nanophased Fe/Ag solid mixture. The as-prepared material, as well as the reduced mixture, is analyzed by various conventional methods. Magnetization loops, ESR, Mössbauer, and magnetoresistance measurements are also conducted to determine the magnetic properties of the products.     

Effect of annealing temperature on the microstructure and optical–electrical properties of Cu–Al–O thin films

We have successfully prepared Cu–Al–O thin films on silicon (100) and quartz substrates by radio frequency (RF) magnetron sputtering method. The as-deposited Cu–Al–O film is amorphous in nature and post-annealing treatment in argon ambience results in crystallization of the films and the formation of CuAlO₂. The annealing temperature plays an important role in the surface morphology, phase constitution and preferred growth orientation of CuAlO₂ phase, thus affecting the properties of the film. The film annealed at 900 °C is mainly composed of CuAlO₂ phase and shows smooth surface morphology with well-defined grain boundaries, thus exhibiting the optimum optical–electrical properties with electrical resistivity being 79.7 Ω·cm at room temperature and optical transmittance being 80% in visible region. The direct optical band gaps of the films are found in the range of 3.3–3.8 eV depending on the annealing temperature.     

Various properties of sputter-deposited Ta–Ru thin films

This paper discusses several structural, electrical and oxidation characteristics of co-sputtered Ta–Ru alloy films on oxidized Si-substrates. From X-ray examination, the Ta₁Ru₁ phase has formed and dominates in the compositions exceeding 54 at.% Ru content. The resistivity of the Ta–Ru thin films can reach a maximum of ∼320 μΩ cm in the composition range between 35 and 54 at.% Ru. After thermal treatment in air (600°C, 1 h), Ru-rich samples show a less increase in resistivity than Ta-rich ones. The observed preferential oxidation of Ta in the Ta–Ru samples can be further interpreted by thermodynamic calculations. The Ta-rich surface oxide is believed to be responsible for the passivating ability of the Ru atom toward oxidation at high temperatures. This results in the Ru of the metallic state though the oxidation of Ta occurs.     

Phase composition and magnetic structure in nanocrystalline ferromagnetic Fe–N–O films

The chemical and phase compositions and structure of the Fe–N–O films produced by reactive dc magnetron sputtering (in Ar or Ar + N₂ gas mixture atmospheres) under different conditions (energy parameters of magnetron, residual pressure in the magnetron chamber after preliminary pumping, operating pressure in gas mixture) have been investigated by energy-dispersive X-ray spectroscopy, X-ray diffraction analysis, and vibrating sample magnetometry. Impurity of nitrogen and oxygen, which are present in the sputtered films, participate in the formation of their phase composition and determine its features. Some phenomena inherent in the nanocrystalline films in the metastable state were found. These are the formation of supersaturated bcc interstitial αFe-based solid solution and precipitation of α’ nitrous martensite with bct crystal lattice. The magnetic structure of the Fe–N–O films, which is characterized by the existence of stochastic domains discovered by correlation magnetometry method, is discussed in terms of the random anisotropy model. It was found that two modes of the magnetic anisotropy field of stochastic domains are formed, which determine the existence of two modes of the coercive field found in the magnetic hysteresis loops.     

Microstructure of soft magnetic FeCo–O(–Zr) films with high saturation magnetization

The effect of microstructure on the soft magnetic properties of (Fe_0.65Co_0.35)_100−x−yZr_xO_y (0⩽x⩽4, 0⩽y⩽14) films has been studied using X-ray diffraction analysis, conventional and high-resolution transmission electron microscopy, and small angle X-ray scattering techniques. The results have shown that good soft magnetic properties are associated with nanoscale grains of the α-Fe(Co) phase. The introduction of oxygen and zirconium to an Fe_0.65Co_0.35 film caused refinement of the microstructure. When the concentration of oxygen and zirconium was low (⩽9 at%), oxide particles (CoFe₂O₄) were embedded in α-Fe(Co) grains. A higher concentration of oxygen and zirconium changed the crystalline oxide to an amorphous oxide, resulting in the formation of smaller grains of the α-Fe(Co) phase. Annealing the Zr-free (Fe_0.65Co_0.35)₉₉O₁ film caused a drastic decrease in the coercivity, the reasons for which have been discussed based on the microstructural observations.     

Magnetoresistance and magnetic properties of Fe3O4 nanoparticle compacts

In this paper,we report on the magnetic properties of Fe3O4 nanoparticles with different grain sizes under different pressures.In all the samples,the saturated magnetization Ms shows a linear decrease with increasing pressure.The thickness of the magnetic dead layer on the nanoparticle surface nuder different pressures was roughly estimated,which also increases with increasing pressure.The transport measurements of the nanoparticle Fe3O4 compacts show that the low-field magnetoresistance (MR) value is insensitive to the grain size in a wide temperature range;however,the high-field MR value is dependent on grain size,especially at low temperatures.These experimental results can be attributed to the different surface states of the nanoparticles.     

Nanostructure and thermal-optical properties of vanadium dioxide thin films

A novel nanopolycrystalline structure of vanadium dioxide thin films is deposited on silicon or fused silica substrates by reactive ion sputtering and followed by an annealing. The characteristic analysis shows that the films have a columnar nanostructure with an average grain of 8 nm. The resistivities as a function of ambient temperatures tested by four-point probes for as-deposited films present that the transition temperature for nanostructure of vanadium dioxide films is near 35 ℃ which lowers about 33 ℃ in comparison with the transition temperature at 68 ℃ in its microstructure.