Structure and magnetic properties of Nb-doped FeZrB soft magnetic alloys

Structure and magnetic properties of Nb-doped (FeZrB)_100−xNb_x alloy are investigated by X-ray diffraction (XRD), differential scanning calorimetry and vibrating sample magnetometer. The fully amorphous structure of the as-quenched ribbons is confirmed by the XRD pattern. With increasing Nb, the glass transition temperature and the onset crystallization temperature are increased, indicating increased stability of the amorphous structure. For x=1, the saturation magnetization of the ribbons is 125.7 emu/g and the optimized annealing temperature increases from 550 to 630 °C. The morphology of the crystallized phases is observed by scanning electron microscopy. The results show that nanocrystalline α-Fe grains are dispersed in the amorphous matrix.     

Microstructure evolution in the rapidly quenched Fe78Si9B13 ribbons

We report microstructure evolution in as-spun Fe₇₈Si₉B₁₃ ribbons under various wheel speeds (s), which was investigated by X-ray diffraction (XRD), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). With decreasing s, the volume fraction of the residual amorphous phase (V_a) in the as-spun ribbons decreases gradually, and the total exothermic heat of the crystallization in the DSC curves also decreases, but the ratio of the exothermic heat of the second crystallization to the first one is on the contrary. α-Fe is found in the ribbon with s of 32.9 m/s, while α-Fe, eutectic α-Fe+Fe₂B, and Fe₃Si phases are found in ribbons with s of 25.6 and 18.3 m/s. The phase precipitating behavior in cooling processes is well consistent with the annealing process in the literatures.     

Influence of Nb substitution for Fe on the magnetic and magneto-impedance properties of amorphous and annealed Fe76.5−xSi13.5B9Cu1Nbx (x=0–7) ribbons

We report a systematic study of the influence of Nb substitution for Fe on the magnetic properties and magneto-impedance (MI) effect in amorphous and annealed Fe_76.5−xSi_13.5B₉Cu₁Nb_x (x=0, 1, 2, 3, 4, 5, 6, and 7) ribbons. The amorphous ribbons were annealed at different temperatures ranging from 530 to 560 °C in vacuum for different annealing times between 5 and 20 min. We have found that for the as-quenched amorphous ribbons, the substitution of Nb for Fe first increases the saturation magnetization (M_s) and decreases the coercivity (H_c) until x=3, for which the largest M_s∼152 emu/g and the smallest H_c∼1.3 Oe are obtained, then an opposite trend is found for x>3. The largest MI ratio (ΔZ/Z∼38% at f=6 MHz) is achieved in the amorphous ribbon with x=3. A similar trend has been observed for the annealed ribbons. The most desirable magnetic properties (M_s∼156 emu/g and H_c∼1.8 Oe) and the largest MI ratio (ΔZ/Z∼221% at f=6 MHz) are achieved for the x=3 sample annealed at 540 °C for 15 min. A correlation between the microstructure, magnetic properties, and MI effect in the annealed ribbons has been established.     

Magnetic properties and domain structures of FeSiB thin films

Smooth Fe₇₈Si₁₀B₁₂ thin films were prepared by r.f. sputtering with the very slow deposition rate of 0.59 nm/min. The as-deposited films were not fully amorphous, instead α-Fe(Si) nanocrystallites were found to be embedded in the amorphous matrix. The saturation magnetostriction λ_s of the as-deposited film is about 6.5 × 10⁻⁶. After annealing at 540 °C for 1 h in an ultrahigh vacuum (4.5 × 10⁻⁵ Pa), the fraction of α-Fe(Si) crystalline phase largely increased, and correspondingly the λ_s decreased to 4.5 × 10⁻⁷. Ripple domain structures were observed in the as-deposited film, while dense stripe domains were observed in the annealed sample, characterized by a very narrow domain width of 80 nm. (1 1 0) texture and island-like configuration of α-Fe(Si) nanocrystallites formed by the annealing treatment are responsible for the perpendicular anisotropy. For the as-deposited film, the magnetization curves increased linearly with the increase of the magnetic field, and showed the very small hysteresis. On the other hand, the annealed sample clearly showed a very steep jump near the origin, which is due to the switch process of the dense stripe domain.     

Recoilless fraction, structural, magnetic and thermal properties of Fe73.5Cu1Nb3Si13.5B9 alloy

Differential scanning calorimetry, X-ray diffraction and room temperature Mössbauer spectrum measurements of Fe_73.5Cu₁Nb₃Si_13.5B₉ (Finemet) alloy have been carried out in order to study its structural and magnetic properties as a function of annealing temperature. The DSC profile of as-quenched Finemet showed two exothermic peaks at 530 and 702 °C, corresponding to two crystallization processes. The Finemet alloy remains amorphous at 450 °C with one broad peak in XRD pattern and one broad sextet in Mössbauer spectrum. When the Finemet alloy was annealed at 550 °C, only well indexed body-center-cubic phase was detected. After being annealed at 650 and 750 °C, the XRD patterns showed the coexistence of α-Fe(Si) and Fe-B intermetallic phases with the increase in XRD peak intensities, indicating the growth of crystallites and the decomposition of Fe_73.5Cu₁Nb₃Si_13.5B₉ alloy at elevated temperatures. The Mössbauer spectra of annealed Finemet alloy could be fitted with 4 or 5 sextets and one doublet at higher annealing temperatures, revealing the appearance of different crystalline phases corresponding to the different Fe sites above the crystallization temperature. The appearance of the nanocrystalline phases at different annealing temperatures was further confirmed by the recoilless fraction measurements.     

The existence of giant magnetocaloric effect and laminar structure in Fe73.5−xCrxSi13.5B9Nb3Cu1

Amorphous soft magnetic ribbons Fe_73.5−xCr_xSi_13.5B₉Nb₃Cu₁ (x=1–5) have been fabricated by rapid quenching on a single copper wheel. The differential scanning calorimetry (DSC) patterns showed that the crystallization temperature of α-Fe(Si) phase is ranging from 542 to 569 °C, a little higher than that of pure Finemet (x=0). With the same annealing regime, the crystallization volume fraction as well as the particle size of α-Fe(Si) crystallites decreased with increasing Cr amount substituted for Fe in studied samples. Especially, the interesting fact is that the laminar structure of heat-treated ribbons on the surface contacted to copper wheel in the fabricating process has been firstly discovered and explained to be related to the existence of Cr in studied samples. The hysteresis loop measurement indicated that there is the pinning of displacement of domain walls. The giant magnetocaloric effect (GMCE) has been found in amorphous state of the samples. After annealing, the soft magnetic properties of investigated nanocomposite materials are desirably improved.     

The influence of substrate temperature and annealing on the properties of pulsed laser-deposited YIG films on fused quartz substrate

Yttrium iron garnet (YIG) thin films were deposited on fused quartz substrate at different substrate temperatures (T_s) varying from room temperature (RT) to 850 °C using pulsed laser deposition (PLD) technique. All the films in the as-deposited state were X-ray amorphous and non-magnetic at RT. The film deposited at RT after annealing at temperatures T_a?700 °C showed both X-ray peaks and the magnetic order. The films deposited at higher T_s (500–850 °C) and then annealed at 700 °C resulted in better-quality films with higher 4πM_s value. The highest value of magnetization was for the sample deposited at 850 °C and annealed at 700 °C, which is 68% of the bulk 4πM_s value.     

Annealing temperature effect on microstructure,magnetic and microwave properties of Fe-based amorphous alloy powders

Fe₇₄Ni₃Si₁₃Cr₆W₄ amorphous alloy powders were annealed at different temperature (T) for 1.5 h to fabricate the corresponding amorphous and nanocrystalline powders. The influences of T on the crystalline structure, morphology, magnetic and microwave electromagnetic properties of the resultant samples were investigated via X-ray diffraction, scanning electron microscopy, vibrating sample magnetometer and vector network analyzer. The results show that the powder samples obtained at T of 650 °C or more are composed of lots of ultra-fine α-Fe(Si) grains embedded in an amorphous matrix. When T increases from 350 to 750 °C, the saturated magnetization and coercivity of the as-annealed powder samples both increase monotonously whereas the relative real permittivity shows a minimal value and the relative real permeability shows a maximal value at T of 650 °C. Thus the powder samples annealed at 650 °C show optimal reflection loss under −10 dB in the whole C-band. These results here suggest that the annealing heat treatment of Fe-based amorphous alloy is an effective approach to fabricate high performance microwave absorber with reasonable permittivity and large permeability simultaneously via adjusting T.     

Effects of high-temperature annealing on magnetic properties of V-doped GaN thin films grown by MOCVD

Metal organic chemical vapor deposition (MOCVD) has been used to grow vanadium-doped GaN (GaN:V) on c-sapphire substrate using VCl₄ as the V source. The as-grown GaN:V exhibited a saturated magnetic moment (M_s) of 0.28 emu/cm³ at room temperature. Upon high-temperature annealing treatment at 1100 °C for 7 min under N₂ ambient, the M_s of the GaN:V increased by 39.28% to 0.39 emu/cm³. We found that rapid thermal annealing leads to a remarkable increase in surface roughness of the V-doped GaN as well as the electron concentration. The annealing also leads to a significant increase in the Curie temperature (T_C), we have identified Curie temperatures about 350 K concluded from the difference between the field-cooled and zero-field-cooled magnetizations. Structure characterization by x-ray diffraction indicated that the ferromagnetic properties are not a result of secondary magnetic phases.     

Effects of rapid thermal annealing on structural, magnetic and optical properties of Ni-doped ZnO thin films

XPS depth profiles were used to investigate the effects of rapid thermal annealing under varying conditions on the structural, magnetic and optical properties of Ni-doped ZnO thin films. Oxidization of metallic Ni from its metallic state to two-valence oxidation state occurred in the film annealed in air at 600 °C, while reduction of Ni²⁺ from its two-valence oxidation state to metallic state occurred in the film annealed in Ar at 600 and 800 °C. In addition, there appeared to be significant diffusion of Ni from the bottom to the top surface of the film during annealing in Ar at 800 °C. Both as-deposited and annealed thin films displayed obvious room temperature ferromagnetism (RTFM) which was from metallic Ni, Ni²⁺ or both with two distinct mechanisms. Furthermore, a significant improvement in saturation magnetization (M_s) in the films was observed after annealing in air (M_s = 0.036 μ_B/Ni) or Ar (M_s = 0.033 μ_B/Ni) at 600 °C compared to that in as-deposited film (M_s = 0.017 μ_B/Ni). An even higher M_s value was observed in the film annealed in Ar at 800 °C (M_s = 0.055 μ_B/Ni) compared to that at 600 °C mainly due to the diffusion of Ni. The ultraviolet emission of the Ni-doped ZnO thin film was restored during annealing in Ar at 800 °C, which was also attributed to the diffusion of Ni.     

Synthesis of α-Fe2O3 nanobelts and nanoflakes by thermal oxidation and study to their magnetic properties

α-Fe₂O₃ nanobelts and nanoflakes have been successfully synthesized by oxidation of iron-coated ITO glass in air. The X-ray diffraction, Raman spectrum and scanning electron microscopy are carried out to characterize the nanobelts and nanoflakes. The formation mechanism has been presented. Significantly, the magnetic investigations show that the magnetic properties are strongly shape-dependent. The magnetization measurements of belt-like and flake-like α-Fe₂O₃ in perpendicular exhibit ferromagnetic feature with the coercivity (H_c) and saturation magnetization (M_s) of 334.5 Oe and 1.35 emu/g, 239.5 Oe and 0.12 emu/g, respectively. For the parallel, belt-like and flake-like α-Fe₂O₃ also exhibit ferromagnetic feature with the H_c and M_s of 205.5 Oe and 1.44 emu/g, 159.6 Oe and 0.15 emu/g, respectively.     

Heat treatment effects on microstructure and magnetic properties of Mn-Zn ferrite powders

Mn-Zn ferrite powders (Mn_0.5Zn_0.5Fe₂O₄) were prepared by the nitrate-citrate auto-combustion method and subsequently annealed in air or argon. The effects of heat treatment temperature on crystalline phases formation, microstructure and magnetic properties of Mn-Zn ferrite were investigated by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning electron microscopy and vibrating sample magnetometer. Ferrites decomposed to Fe₂O₃ and Mn₂O₃ after annealing above 550 °C in air, and had poor magnetic properties. However, Fe₂O₃ and Mn₂O₃ were dissolved after ferrites annealing above 1100 °C. Moreover, the 1200 °C annealed sample showed pure ferrite phase, larger saturation magnetization (M_s=48.15 emu g⁻¹) and lower coercivity (H_c=51 Oe) compared with the auto-combusted ferrite powder (M_s=44.32 emu g⁻¹, H_c=70 Oe). The 600 °C air annealed sample had the largest saturation magnetization (M_s=56.37 emu g⁻¹) and the lowest coercivity (H_c=32 Oe) due to the presence of pure ferrite spinel phase, its microstructure and crystalline size.     

Structural transformations of Fe81B13Si4C2 amorphous alloy induced by heating

Thermal stability and crystallization of the Fe₈₁B₁₂Si₄C₂ alloy were investigated in the temperature range 25-700 °C by the XRD and Mössbauer analysis. It was shown that on heating the as-prepared amorphous Fe₈₁B₁₂Si₄C₂ alloy undergoes thermal stabilization through a series of structural transformations involving the process of stress-relieving (temperature range 200-400 °C), followed by a loss of ferromagnetic properties (Curie temperature at 420 °C) and finally crystallization (temperature range 450-530 °C). The process of crystallization begins by formation of two crystal phases: Fe₃B and subsequently Fe₂B, as well as a solid solution α-Fe(Si). With increase in annealing temperature, the completely crystallized alloy involved only two phases, Fe₂B and solid solution α-Fe(Si).XRD patterns established a difference in phase composition and size of the formed crystallites during crystallization depending on the side (fishy or shiny) of the ribbon. The first nuclei of the phase α-Fe₃Si were found on the shiny side by XRD after heat treatment even at 200 °C but the same phase on the fishy side of ribbon was noticed after heat treatment at 450 °C. The largest difference between the contact and free surface was found for the Fe₂B phase crystallized by heating at 700 °C, showing the largest size of crystallites of about 130 nm at 700 °C on the free (shiny) surface.     

Synthesis, structural and magnetic properties of the nanocomposite Fe63B23Nd7Y3Nb3Cr1 magnets

The Fe₆₃B₂₃Nd₇Y₃Nb₃Cr₁ nanocomposite magnets in the form of sheets have been prepared by copper mold casting technique. The phase evolution, crystal structure, microstructural and magnetic properties have been investigated in the as-cast and annealed states. The as-cast sheets show magnetically soft behaviors which become magnetically hard by thermal annealing. The optimal annealed microstructure was composed of nanosize soft magnetic α-Fe (19-29 nm) and hard magnetic Nd₂Fe₁₄B (45-55 nm) grains. The best hard magnetic properties such as intrinsic coercivity, _jH_c of 1119 kA/m, remanence, B_r of 0.44 T, magnetic induction to saturation magnetization ratio, M_r/M_s=0.61 and maximum energy product, (BH)_max of 55 kJ/m³ was obtained after annealing at 680 °C for 15 min. The annealing treatment above 680 °C results in non-ideal phase grains growth, which degrade the magnetic properties.     

Simultaneous variations of microstructure and magnetic properties of Ni58Fe12Zr20B10 nanostructure/amorphous alloy prepared by mechanical alloying

This study aims to evaluate magnetic and micro-structural properties of amorphous/nanocrystalline mechanically alloyed Ni₅₈Fe₁₂Zr₂₀B₁₀ powders with ball-milling time up to 190 h. Structural, micro-structural and thermal evaluations of the milled powders were carried out by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and differential scanning calorimetry (DSC) methods. Magnetic properties were also measured by a vibrating sample magnetometer (VSM) instrument. Results showed that the amorphous phase reached maximum value of 95% and the crystallite size was about 3 nm at the end of the milling. Magnetization saturation (M_s) decreased slightly and coercivity (H_c) reached to the highest value at 72 h of the milling time. At the 190 h of milling, the coercivity and saturation magnetization reached 18 Oe and 20 emu/g, respectively. While, after an appropriate amount of heat treatment, these two variables became approximately 2 Oe and 32 emu/g.     

Curie temperatures and crystallization behavior of amorphous Fe81−xNixZr7B12 (x=10, 20, 30, 40, 50, 60) alloys

Curie temperature, crystal structure and crystallization behavior of amorphous alloys with the stoichiometry Fe_81−xNi_xZr₇B₁₂ (x=10–60) have been studied by X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and AC-magnetization (TMAG) measurements as functions of temperature. The thermal stability of long-range magnetic order, T_C vs. Ni content in as-quenched amorphous alloys exhibits maximum at 352 °C for x=40. The primary crystallization has been detected during annealing at the first crystallization stage of all ribbons investigated.     

Magnetic properties and static-dynamic magnetostrictive characteristics for SmFe2/Fe exchange-coupled multilayers

Giant magnetostrictive SmFe₂/Fe exchange-coupled multilayers were fabricated by ion beam sputtering deposition on glass substrates. The effects of SmFe₂/Fe exchange coupling action and vacuum annealing on soft-magnetic property and static-dynamic magnetostrictive characteristics of SmFe₂/Fe multilayers were investigated. The results showed that the soft-magnetic, static-dynamic magnetostrictive characteristics were greatly improved by SmFe₂/Fe exchange coupling action and proper vacuum annealing treatment temperature. Compared with that of SmFe₂ single film, the coercivity in the direction of easy magnetization axis for SmFe₂/Fe exchange-coupled multilayers exhibited a greater decrease. Better soft-magnetic properties were achieved (H_c=2.54 kA/m, M_s=120.38 emu/g, and M_r/M_s=0.21) after vacuum annealing at certain temperature. The magnetostrictive coefficient for SmFe₂/Fe exchange-coupled multilayers was about 135 ppm at 16 kA/m magnetic field. At first order resonant frequency (99.2 Hz), the amplitude peak-peak value for the as-deposited SmFe₂/Fe exchange-coupled multilayers was 46 μm. After the vacuum annealing treatment at 250 °C, the amplitude peak-peak value increased to 650 μm.     

Effect of pH value on the structural and magnetic properties of nanocrystalline strontium hexaferrite thin films

Strontium hexaferrite SrFe₁₂O₁₉ thin films have been synthesized at different pH, adjusted by NH₄OH, on the Si (1 0 0) substrate using a spin coating sol-gel process. Fourier transform infrared spectroscopy analysis and theoretical calculations were conducted for determination and controlling metal citrates in solution precursors. X-ray diffraction, scanning electron microscopy and vibrating sample magnetometer were applied to evaluate the composition, microstructure, crystallite size and magnetic properties of the SrFe₁₂O₁₉ thin films. Using the solution with pH 7, the approximately single phase strontium hexaferrite thin films with optimum physical properties can be obtained at calcination temperature of 800 °C. The SrFe₁₂O₁₉ thin films derived from the solution with pH 7 after calcination at 800 °C exhibited crystallite size of 42 nm and magnetic properties of M_s=267 emu/cm³ (at 10 kOe), M_r=134 emu/cm³ and H_c=4290 Oe.     

Magnetic properties of cobalt substituted M-type barium hexaferrite prepared by co-precipitation

The co-precipitation and solid state methods were used in the synthesis of barium hexaferrite (BaM). Phase pure BaM was obtained with 1, 2, 3, 5, 10, 15, 20 and 30 wt% cobalt oxide (Co₃O₄). The addition of Co^2+/3+ ions to the BaM increased the permeability and magnetic loss tangent to a value of 3.5 at 5% and reduced to 1 at 30% doping. With increased Co doping, M_s was reduced from 87-58 emu/g, M_r increased from 11 to 40 emu/g with 3–5 wt% Co and 9 emu/g for 30% doping. H_c sharply increased from 540 to 2200 Oe with a reduction to 280 Oe at 10 K with increasing temperature to 300 K. T_c increased from 740 to 750 K for 30% Co doping. DTA–TGA studies of green body showed decarboxilation to occur at around 825 °C and the transformation of residual Co₃O₄ to Co₂O₃ at around 577 °C. The XRD data confirmed the Co ions substituting into Fe sites until a 10–15% doping level where the structure altered to W-type hexaferrite. The densities of the compounds varied with doping to a maximum of 4.45 g/cm³.     

Synthesis and characterization of lithium ferrite by oxalate precursor route

Nanocrystalline lithium ferrite (LiFe₅O₈) powders have been synthesized by oxalate precursor route. The effects of Fe³⁺/Li⁺ mole ratio, and annealing temperature on the formation, crystalline size, morphology and magnetic properties were systematically studied. The Fe³⁺/Li⁺ mole ratio was controlled from 5 to 3.33 while the annealing temperature was controlled from 600 to 1100 °C. The resultant powders were investigated by differential thermal analyzer (DTA), X-ray diffractometer (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). DTA results showed that LiFe₅O₈ phase started to form at around 520 °C. XRD indicated that LiFe₅O₈ phase always contained α-Fe₂O₃ impurity and the hematite phase formation increased by increasing the annealing temperature ?850 °C for different Fe³⁺/Li⁺ mole ratios 5, 4.55 and 3.85. Moreover, lithium ferrite phase was formed with high conversion percentage at critical annealing temperature 750–800 °C. Single well crystalline LiFe₅O₈ phase was obtained at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperatures from 800 to 1000 °C. Maximum saturation magnetization (68.7 emu/g) was achieved for the formed lithium ferrite phase at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperature 1000 °C.