Structure and magnetic properties of (Nd,Dy)16(Fe,Co)76−xTixB8 powders prepared by mechanical alloying

Nanocrystalline (Nd,Dy)₁₆(Fe,Co)_76−xTi_xB₈ magnets were prepared by mechanical alloying and respective heat treatment at 973–1073 K/30–60 min. An addition of 0.5 at % of Ti results in an increase of coercivity from 796 to 1115 kA m⁻¹. Partial substitution of Nd by Dy results in an additional increase of coercivity up to 1234 kA m⁻¹. Mössbauer investigations shows that for x?1 the (Nd,Dy)₁₆(Fe,Co)_76−xTi_xB₈ powders are single phase. For higher Ti contents (x>1) the mechanically alloyed powders heat treated at 973 K are no more single phase, and the coercivity decreases due to the presence of an amorphous phase. A heat treatment at a higher temperature (1073 K) for longer time (1 h) results in the full recrystallisation of powders. The mean hyperfine field of the Nd₂Fe₁₄B phase decreases for titanium contents of 0?x?1, and remains constant for x>1. This indicates that the Ti content in the Nd₂Fe₁₄B phase reaches its maximum value.     

Anisotropic powder from sintered NdFeB magnets by the HDDR processing route

Sintered NdFeB-based scrap magnets were recovered and processed using the HD and HDDR routes. The effects of varying the HDDR processing temperature were investigated (over the range 835-930 °C). The disproportion was carried out with a pressure ramp to a maximum of 1000 mbar hydrogen pressure with a 1 h hold time at each step and the optimum recombination conditions were set at 100 mbar with a 20 min hold time. Anisotropic NdFeB powder was produced in all cases with the best magnetic properties achieved at a processing temperature of 880 °C, producing powder with a remanence of 1.10(±0.02) T and an intrinsic coercivity of 800 (±16) kA m⁻¹ and giving a (BH)_max of 129(±2.5) kJ m⁻³.     

Effect of Co underlayer on soft magnetic properties and microstructure of FeCo thin films

High saturation magnetization soft magnetic FeCo (=Fe₆₅Co₃₅) films were prepared using a thin Co underlayer. The FeCo/Co films exhibited a well-defined in-plane uniaxial anisotropy with easy axis coercivity (H_ce) of 10 Oe and hard axis coercivity (H_ch) of 3 Oe, and a half reduction of H_c with H_ce=4.8 Oe and H_ch=1.0 Oe was obtained when the composition was adjusted to 25 at% Co. The effective permeability of the films remains flat around 250 to 800 MHz. The saturation magnetostriction was 5.2×10⁻⁵ and the intrinsic stress was 0.8 GPa in FeCo single layer, both were slightly reduced by Co underlayer. The Co underlayer changed the preferred orientation of the FeCo films from (2 0 0) to (1 1 0) but more significantly, reduced the average grain size from ∼74 to ∼8.2 nm. It also reduced the surface roughness from 2.351 to 0.751 nm. The initial stage and interface diffusion properties were examined by TEM and XPS.     

Preparation, characterization and magnetic properties of the doped barium hexaferrites BaFe12−2xCox/2Znx/2SnxO19, x=0.0-2.0

A series of powders of M-typed barium hexaferrites doped with Co, Zn and Sn of general formula BaFe_12-2xCo_x/2Zn_x/2Sn_xO₁₉ (x=0-2.0) were prepared by the co-precipitation/molten salt method. The structures, particle morphology and magnetic properties of the products were characterized by X-ray powder diffraction, vibrating sample magnetometer and ESEM/EDX. The results show that the crystallinity of the samples decreases with increase in the doping amount x. When x is less than 0.6, it is possible to obtain perfectly crystallized hexagonal BaFe_12-2xCo_x/2Zn_x/2Sn_xO₁₉, where the diameters of the particles are around 500 nm. The saturation magnetization of pure barium ferrite BaFe₁₂O₁₉ produced with this method is 71.9 A m² kg⁻¹ at room temperature and the intrinsic coercivity (H_c) is 367.8 kA m⁻¹. The doped barium hexaferrite powder obtained when x is between 0.3 and 0.4 exhibits high saturation magnetization and a temperature dependence of coercivity close to zero.     

Production and corrosion resistance of NdFeBZr magnets with an improved response to thermal variations during sintering

This study describes an attempt to produce NdFeB magnets that are insensitive to the sintering temperature. It was found that addition of Zr to NdFeB magnets significantly augmented the thermal stability of this magnetic material during sintering at high temperature even at industrial scale. The best sintered magnets were produced by jet-milling the powder (to achieve an average 3.4 μm particle size), and then aligned, pressed and sintered under argon at 1100 °C for 3 h followed by appropriate heat treatment. The magnetic properties of the resulting magnets were: (BH)_m=403.8 kJ m⁻³ (±4.7 kJ m⁻³), B_r=1430 mT (±9 mT) and _iH_c=907 kA m⁻¹ (±12 kA m⁻¹). Large grain growth, in excess of 100 μm in the Zr-free magnets, was observed during sintering at 1100 °C. This did not occur in the presence of Zr. These observations imply that the sensitivity of this class of magnets to high sintering temperatures is greatly reduced by Zr addition. Corrosion resistance of NdFeB was therefore significantly improved by the addition of small amounts of Zr.     

Preference orientation and magnetic properties of CoxFe3−xO4 nanocrystalline thin films on quartz substrate

Nanocrystalline spinel ferrite thin films of Co_xFe_3−xO₄ (x=0.3$x=0.3$, 0.5, 0.8, and 1.0) have been prepared by RF sputtering on quartz substrate without a buffer layer at room temperature and annealed at the temperature range from 200 to 600 °C in air. The as-sputtered films exhibit the preferred orientation and the high magnetization and coercivity. After annealing, the preferred orientations become poor, but the magnetization and coercivity increase. The sample with a magnetization of 455 emu/cm³, a coercivity of 2.8 kOe, a remanence ratio of 0.72, and a maximum energy product of 2.4 MGOe has been obtained. The influence of Co ions and annealing temperature on the magnetic properties has been discussed.     

Effect of Cr100−xTix (x = 0-19 at.%) alloy underlayers on the high coercivity of FePt thin film below the substrate temperature of 250 °C

The effect of Cr_100−xTi_x underlayer on orderd-L1₀ FePt films was investigated. A low-temperature ordering of FePt films could be attained through changing the Ti content of Cr_100−xTi_x underlayer. The ordering temperature of the 30 nm FePt film grown on 20 nm Cr₉₀Ti₁₀ underlayer was reduced to 250 °C which is practical manufacture process temperature. An in-plane coercivity was very high to 6000 Oe and a ratio of remnant magnetization (M_r) to saturation magnetization (M_s) was as large as 0.85. This result indicates that the coercivity obtained at 250 °C by the effect of CrTi underlayer is significantly higher than those obtained at 250-275 °C by the effect of underlayers in other conventional studies. The prominent improvement of the magnetic properties of ordered FePt thin films at low temperature of 250 °C could be understood with considering the strain-induced ordering phase transformation associated with lattice mismatch between Cr underlayer and FePt magnetic layer due to an addition of Ti content.     

Thin films of semiconducting lithium ferrite produced by pulsed laser deposition

Thin films of lithium ferrite (Li_0.5Fe_2.5O₄) have been deposited on (0 0 1) Al₂O₃ by pulsed laser deposition, with substrate deposition temperatures ranging between 500 and 800 °C, and oxygen pressures between 1 × 10⁻¹ and 4 × 10⁻⁷ mbar. X-ray diffraction shows that films grow with a (1 1 1) orientation. Conversion electron Mössbauer spectra for the high-pressure films show a single sextet with a hyperfine field of 49 T, while the low-pressure films show two sextets with hyperfine fields of 47 and 49 T. The spectra also reveal paramagnetic ferric iron in both types of films. Magnetization measurements of the films show a saturation magnetization of between 1.7 and 3.1μ_B per formula unit and a coercivity of between 10 and 44 mT. The films prepared under the lower oxygen pressures are semiconducting with resistivities of 2 × 10⁻² to 8 × 10⁻² Ω cm. They exhibit an anomalous Hall effect with p-type conduction at 175 K.     

Structural and magnetic properties of sol-gel Co2xNi0.5−x Zn0.5−xFe2O4 thin films

Nanocrystalline Co_2xNi_0.5−xZn_0.5−xFe₂O₄ (x=0−0.5) thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology as well as magnetic and microwave absorption properties of the films calcined at 1073 K were studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. All films were uniform without microcracks. The Co content in the Co-Ni-Zn films resulted in a grain size ranging from 15 to 32 nm while it ranged from 33 to 49 nm in the corresponding powders. Saturation and remnant magnetization increased with increase in grain size, while coercivity demonstrated a drop due to multidomain behavior of crystallites for a given value of x. Saturation magnetization increased and remnant magnetization had a maximum as a function of grain size independent of x. In turn, coercivity increased with x independent of grain size. Complex permittivity of the Co-Ni-Zn ferrite films was measured in the frequency range 2-15 GHz. The highest hysteretic heating rate in the temperature range 315-355 K was observed in CoFe₂O₄. The maximum absorption band shifted from 13 to 11 GHz as cobalt content increased from x=0.1 to 0.2.     

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.     

Magnetic,structural and electrical properties of ordered and disordered Co50Fe50 films

Co₅₀Fe₅₀ films with thickness varying from 100 to 500 Å were deposited on a glass substrate by sputtering process, respectively. Two kinds of CoFe films were studied: one was the as-deposited film, and the other the annealed film. The annealing procedure was to keep the films at 400 °C for 5 h in a vacuum of 5×10⁻⁶ mbar. From the X-ray study, we find that the as-deposited film prefers the CoFe(1 1 0) orientation. Moreover, the body-centered cubic (bcc) CoFe(1 1 0) line is split into two peaks: one corresponding to the ordered body-centered tetragonal (bct) phase, and the other, the disordered bcc phase. After annealing, the peak intensity of the ordered bct phase becomes much stronger, while that of the disordered bcc phase disappears. The annealing has also caused the ordered CoFe(2 0 0) line to appear. When the amount of the ordered bct phase in Co₅₀Fe₅₀ is increased, the saturation magnetization (M_s) and coercivity (H_c) become larger, but the electrical resistivity (ρ) decreases. From the temperature coefficient of resistance (TCR) measurement, we learn that the bct grains in the CoFe film start to grow at temperature 82 °C.     

The influence of pH and bath composition on the properties of Fe-Co alloy film electrodeposition

Fe-Co films were electrodeposited on ITO glass substrates from the electrolytes with different molar ratio of Co²⁺/Fe²⁺ and different pH values (2.1, 2.9, 3.7, and 4.3) at 25 °C. The properties of Fe-Co alloy films depend on both Co²⁺ and Fe²⁺ concentrations in electrolyte and pH values was studied. The content of Co increases from 40% to 85% as the mole ratio of CoSO₄/FeSO₄ increasing from 0.50/0.50 to 0.90/0.10 in electrolyte and slightly decreases from 77% to 63% as the pH values increasing from 2.1 to 4.3. The X-ray diffraction analysis reveals that the structures of the films strongly depend on the Co content in the binary films. The surface morphologies of the films are influenced by the combined action of composition and phase structure. The saturation magnetization reaches a maximum value of 2974.03 emu/cm³ and coercivity reaches a minimum value of 42.72 Oe of the Fe_0.30Co_0.70. The saturation magnetization reaches a maximum values of 2974.03 emu/cm³ and coercivity reaches a minimum values of 42.72 Oe of the Fe_0.30Co_0.70 at pH = 2.9.     

Magnetization reversal process and intrinsic coercivity of sputtered Sm2Co17-based films

The Sm₂Co₁₇-based intermetallic films with additives of Fe, Cu, and Zr have been deposited on Si(1 0 0) substrates by dc magnetron sputtering process. Subsequent thermal treatment and the film thickness are found to have significant contribution to the crystal structure and grain structure, which determines the magnetization reversal process and intrinsic coercivity (H_C) of these films. The conventional thermal annealing (CTA) treatment almost failed to crystallize the as-deposited films, leading to a very low H_C. Continuous and homogeneous domain walls cannot form in this deteriorated microstructure, so that the pinning mechanism can be excluded. Contrarily, the films with thickness exceeding 0.8 μm treated by rapid recurrent thermal annealing (RRTA) show an improved H_C, which is attributed to the observed completed crystallization and compact microstructure. It is suggested that this film structure is responsible for providing continuous and homogeneous domain walls, leading to a magnetization reversal process controlled by domain wall pinning model. In special, the H_C of the RRTA-treated film with thickness of 1.8 μm shows a good temperature dependence from 25 to 300 °C, with intrinsic coercivity temperature coefficient β of −0.23%/°C.     

Magnetic properties of (Nd,Pr)–Fe–B nanocomposite over quenched and annealed ribbons

The base alloys of nominal composition (Nd_0.75Pr_0.25)_yFe_balanceB_x (y=10−9.2 and x=6−19.2) were chosen to study the influence of RE/B ratio, smaller than stochiometric composition on magnetic properties of over quenched and annealed ribbons. From X-ray diffraction analysis of these ribbons, the α-Fe and Fe₃B phases were observed along with (Nd,Pr)₂Fe₁₄B major phase. The average grain size was calculated using these patterns as: 35 nm for α-Fe, 45 nm for (Nd,Pr)₂Fe₁₄B and 22 nm for Fe₃B particles. TEM analysis also supported the nano distribution of the above phases. These X-ray graphs support the idea of exchange coupling between hard and soft phases responsible for the observed magnetic properties. In these ribbons the saturation magnetization J_s and remnant magnetization J_r increases from 1.19 T to 1.66 T and from 0.65 T to 0.91 T, respectively as RE/B ratio increases. The increase in J_s and J_r may be attributed to the presence of exchange coupling between these phases. The corresponding coercivity _jH_c decreases from 673.33 to 271.33 k Am⁻¹. The maximum energy product (BH)_max initially increases from 72.42 kJ m⁻³to 109.85 kJ m⁻³ up to RE/B≈1 and then decreases to 58.5 kJ m⁻³, depending on the shape of second quadrant B–H loop. The coercivity mechanism observed from initial hysteresis curve was considered to be nucleation of domain wall.     

Room-temperature ferromagnetism in Sn1−xMnxO2 nanocrystalline thin films prepared by ultrasonic spray pyrolysis

Sn_1−xMn_xO₂ (x=0.01-0.05) thin films were synthesized on quartz substrate using an inexpensive ultrasonic spray pyrolysis technique. The influence of doping concentration and substrate temperature on structural and magnetic properties of Sn_1−xMn_xO₂ thin films was systematically investigated. X-ray diffraction (XRD) studies of these films reflect that the Mn³⁺ ions have substituted Sn⁴⁺ ions without changing the tetragonal rutile structure of pure SnO₂. A linear increase in c-axis lattice constant has been observed with corresponding increase in Mn concentration. No impurity phase was detected in XRD patterns even after doping 5 at% of Mn. A systematic change in magnetic behavior from ferromagnetic to paramagnetic was observed with increase in substrate temperature from 500 to 700 °C for Sn_1−xMn_xO₂ (x=0.01) films. Magnetic studies reveal room-temperature ferromagnetism (RTFM) with 3.61×10⁻⁴ emu saturation magnetization and 92 Oe coercivity in case of Sn_1−xMn_xO₂ (x=0.01) films deposited at 500 °C. However, paramagnetic behavior was observed for the films deposited at a higher substrate temperature of 700 °C. The presence of room-temperature ferromagnetism in these films was observed to have an intrinsic origin and could be obtained by controlling the substrate temperature and Mn doping concentration.     

Preparation and magnetic properties of La-Mn and La-Co doped barium hexaferrites prepared via an improved co-precipitation/molten salt method

La-Mn and La-Co doped barium hexaferrites of formula Ba_(1−x)La_xFe_(12−x)M_xO₁₉ (M=Mn, Co) (x=0.05 to 0.40) were prepared with an improved co-precipitation/molten salt method. For the synthesis, aqueous solutions of the appropriate metal chlorides were prepared in the ratio required except that the initial mole ratio of Fe and dopants to Ba was chosen to be 11:1, and then mixed with excess Na₂CO₃. The solutions were then cooled, filtered off, dried, then mixed with KCl flux, and heated at 450 °C and for 2 h. The temperature was then raised to 950 °C and kept for 4 h, then cooled. This new synthesis method, which employs a lower temperature and shorter reaction time, gives products with improved crystallinity and purity while the saturation magnetization and coercivity values are comparable with those synthesized via the high temperature method.     

Crystal structure and magnetic properties of hard magnetic Sm2Fe17Nδ thin films with Co substitution

The crystal structure and magnetic properties of the hard magnetic Sm₂(Fe_1−xCo_x)₁₇N_δ thin films prepared by dc magnetron sputtering and subsequent nitrogenation process were investigated. It is found that the N content and crystal structure determine the non-monotonic dependence of the coercivity H_C on nitriding temperature for the films with x=0. With nitriding temperature exceeding 300 °C, N atoms can enter the Sm₂Fe₁₇ phase and the N content increases with increasing nitriding temperature, which leads to an increased coercivity. However, the maximum value of the H_C is observed at 400 °C. The α-Fe soft phase appears with nitriding temperature further increasing to 500 °C, which is responsible for the decreased H_C. When x is between 0 and 0.36, the films exhibit single Th₂Zn₁₇-type structure. Co atoms are found to go into the lattice of the 2:17 phase, generating an enhanced exchange coupling interaction between the nano-grains, which is responsible for the improved hard magnetic properties of the films with Co substitution at a certain range. Especially, the optimal value of the coercivity H_C and remanence ratio M_R/M_S reaches 4.0 kOe and 0.70 for the films with x=0.17 and 0.36, respectively.     

Fabrication and characterization of magnetic Fe3O4-CNT composites

Carbon nanotubes (CNTs) decorated with magnetite nanoparticles on their external surface have been fabricated by in situ solvothermal method, which was conducted in benzene at 500 °C with ferrocene and CNTs as starting reagents. The as-prepared composites were characterized using XRD, FTIR, SEM and TEM. It has been found that the amount of magnetite nanoparticles deposited on the CNTs can be controlled by adjusting the initial mass ratio of ferrocene to CNTs. The Fe₃O₄-CNT composites display good ferromagnetic property at room temperature, with a saturation magnetization value (M_s) of 32.5 emu g⁻¹ and a coercivity (H_c) of 110 Oe.     

In-plane magnetization with high coercivity in terbium iron garnet thin films deposited on Pt/Si substrate by PLD

We report on the growth of terbium iron garnet (TbIG, Tb₃Fe₅O₁₂) thin films having anomalously large coercivity and in-plane easy axis of magnetization. The TbIG thin films were prepared at room temperature (RT) on Pt/Si(1 0 0) substrates by pulsed laser deposition technique. The films deposited at RT were X-ray amorphous and do not show any magnetic order. Annealing of the RT deposited film at 900 °C resulted into fully textured (532) TbIG film. Atomic force microscopy and cross-sectional scanning electron microscopy studies of the TbIG films showed good surface quality with an average surface roughness of 5.0 nm and thickness of about 300 nm, respectively. The M-H loops measured at 20 K for TbIG films, exhibit about an order of magnitude enhancement in the coercivity value (H_c) than the single crystal. In-plane and out-of-plane M-H loops revealed that the easy axis of the magnetization lies within the film’s plane. In-plane magnetization combining with large H_c value of the TbIG thin film may be of scientific interest for the possible applications.     

The influence of Nd-Co substitution on the magnetic properties of non-stoichiometric strontium hexaferrite nanoparticles

Non-stoichiometric Nd-Co substituted hexaferrites of composition Sr_1−xNd_xFe_12(1−x)Co_xO₁₉ (x=0-0.4) were prepared by the self-propagating combustion method and subsequent heat treatments. Structural characterization of samples showed that the M-type hexagonal structure can be maintained for substitutions x<0.4 without the segregation of secondary phases on samples calcined at 1100 °C. The crystallites sizes range between 50 and 70 nm. Mössbauer spectroscopy results indicate that the iron vacancies are not evenly distributed over the lattice and that Co/Fe substitution mainly takes place in site 4f2. Magnetic measurements reveal that values of saturation magnetization M_S increased from 72 to 76 Am²/kg (x=0-0.2), while coercivity H_c increased from 26.40 to 58.70 A/m (x=0-0.3). Nd-Co substitutions enhance magnetic properties in deficient iron Sr hexaferrites.