The origin of coercivity decrease in fine grained Nd-Fe-B sintered magnets

Microstructures of fine grained Nd-Fe-B sintered magnets that were produced by the pressless process were investigated to understand the origin of the sudden coercivity decrease below a certain grain size. The intrinsic coercivity is inversely proportional to ln D² with the highest coercivity of 17 kOe at D∼4.5 μm, below which the coercivity drops as the grain size decreases. We found that the degradation of the coercivity of the magnet with a grain size of 3 μm was mainly caused by the inhomogeneous distribution of fcc-Nd oxide whose volume fraction increased with respect to the dhcp Nd-rich phase.     

Investigation of the domain structure of sintered Nd-Fe-B permanent magnets by Bitter-pattern method

The conventional Bitter-pattern technique and the colloid-scanning electron microscopy (colloid-SEM) method were used to study the domain structure of polycrystalline sintered Nd-Fe-B permanent magnets. In the thermally demagnetized state most of the grains are multidomain and the domain structures resemble those observed in bulk uniaxial crystals with strong magnetocrystalline anisotropy. Investigations of the magnetic microstructure during magnetizing cycle showed that the domain walls can easily be moved within the grains and that the magnetization reversal in sintered Nd-Fe-B magnets occurs predominantly by the nucleation and expansion of reverse domains at structural imperfections near the grain boundaries. It is also shown that the colloid-SEM method is more surface sensitive and reveals the domain structure with better resolution than the conventional Bitter technique. Thanks to the application of digital image processing systems, clear and high contrast domain images were obtained. The work was supported by the Lódź University within Research Grant 505/694 (2004).     

Structural and magnetic properties of SmCo5.6Ti0.4 alloy

Three series of SmCo_5.6Ti_0.4 samples were prepared by quenching, melt spinning, and ball milling, respectively. Annealing at different temperatures was carried out for the three series. The influence of the processing routes on the structural and magnetic properties was systematically investigated for this alloy. The as-quenched bulk sample consisted of three phases with a rather coarse grain microstructure. Low intrinsic coercivity (_iH_c) of 0.12 T was obtained in this sample. While the as-spun ribbons and as-milled/annealed powders showed the CaCu₅-type phase (1:5) plus Th₂Zn₁₇-type phase (2:17), and the 1:5 phase plus TbCu₇-type phase (1:7), respectively, with nanograin microstructure. The _iH_c of as-spun ribbons and as-milled/annealed (700 °C for 2 h) powders was found to be 0.59 and 2.23 T, respectively. Coercivity mechanism of these as-spun ribbons is mainly of nucleation type. In the as-milled/annealed powders, the network of the nanograin boundaries is believed to provide strong pinning sites for the domain wall movement.     

Magnetic Force Microscopy Study of Alternate Sputtered （001） Oriented L1o Phase FePt Films

We present a magnetic force microscopy study of alternate sputtered （001） oriented L1o phase FePt films. It is found that the root-mean-square value of phase shift of magnetic force images, （ △Ф）rms, can be used to characterize the perpendicular anisotropy for a series of specimens. Therefore, the considerable improvement of the perpendicular anisotropy after post-annealing can be characterized. In addition, the magnetic properties, magnetic and crystalline microstructures before and after post-annealing are compared for the typical [Fe5nm Pt5 nm]10 film with substrate temperature T8 = 500℃, single layer thickness d = 5 nm and total layer thickness D=100 nm to confirm the effect of post-annealing on improving the perpendicular anisotropy for Fe-Pt films.     

Effect of SiO2 nanopowders on magnetic properties and corrosion resistance of sintered Nd-Fe-B magnets

To improve the magnetic properties and corrosion resistance of magnet, SiO₂ nanopowders were added into Nd_28.25Dy_2.75Fe_balAl_0.15Ga_0.1Nb_0.1B_0.98-sintered magnets as grain boundary modifiers. It was found that the intrinsic coercivity (H_cj), remanence (B_r) and corrosion resistance were all improved with addition of certain amount of SiO₂ nanopowders. The optimum addition amount of SiO₂ nanopowders was found to be 0.01 wt%. Thermodynamic calculation in combination of energy dispersive X-ray spectroscopy (EDX) analyses indicated that SiO₂ nanopowders reacted with Nd of Nd-rich phase. As a result, the intergranular phase was modified, and the grain growth of main phase was restrained. It led to the optimization of microstructure.     

Hard magnetic properties of ErCo7−xCux [0.3⩽x⩽1] system

We report the observation of excellent hard magnetic properties on purely single phase ErCo_7−xCu_x compounds with x=0.3, 0.5, 0.8 and 1. Cu substitution leads to a decrease in the saturation magnetization, but enhances the uniaxial anisotropy in this system. The large anisotropy field (∼100 kOe) is attributed to the Er and the Co sublattices. Domain wall pinning effect seems to play a crucial role in determining the temperature and field dependences of magnetization in these compounds. The hard magnetic properties obtained at room temperature (RT) are comparable to the best results obtained in other RCo₇ based materials.     

Structural and magnetic properties of SmCo7−xMox alloys

Phase structure and magnetic properties of the as-cast and as-milled/annealed SmCo_7−xMo_x (x=0, 0.1, 0.2, 0.3, 0.4) alloys have been systematically studied. It is found that all the as-cast series alloys are composed of the CaCu₅-type and Th₂Zn₁₇-type phases. Saturation magnetization of the samples decreases with the Mo content increasing. Intrinsic coercivities (_iH_c) of no more than 0.06 T are observed in these as-cast samples, due to their rather coarse grain microstructures with an average grain size of 50 μm. The as-milled/annealed SmCo_7−xMo_x powders crystallize in the disordered TbCu₇-type (1:7) structure with very fine nanograins, and a minor Co₃Mo phase appears in the samples with x=0.1-0.4. High _iH_c (?0.95 T) are achieved in these samples, with a maximum of 1.26 T located at x=0.2, which can be primarily attributed to strong pinning of the domain wall motion at the nanograin boundaries. The temperature coefficient (β) of the _iH_c is about −0.22%/°C in the temperature range of 25-400 °C for the as-milled/annealed samples.     

Studies on the magnetic properties for single-phase nanocrystalline FePt magnets with different orientation degrees

The single-phase nanocrystalline FePt magnets composed of 343 irregular-shaped grains are built. The demagnetization curves are simulated by micromagnetic finite element method. The remanence, coercivity and maximum energy product of the magnets decrease with deteriorating grain alignment. The characteristics of variation of magnetic properties with the degree of orientation are closely related to the average grain size of nanocrystalline magnets. The contribution of intergrain exchange coupling (IGEC) to remanence enhancement is associated to the degree of orientation, and decreases with improved grain alignment. With decreasing grain size, coercivity increases for anisotropic nanocrystalline magnets, which is completely different from that of isotropic nanocrystalline magnets.     

The role of dipolar interaction in nanocomposite permanent magnets

The effects of dipolar interactions on the magnetization behaviors and magnetic properties of the nanocomposite magnets have been studied by micromagnetic simulations. Numerical results show that the dipolar interaction plays an important role during the demagnetization process, especially in the magnets with large soft-phase content _vs$v_{\mathrm{s}}$. For the isotropic nanocomposites, the remanence enhancement can be controlled through adjustments of the grain size D   and _vs$v_{\mathrm{s}}$. However, the appearance of magnetic vortex state leads to a very low remanence in the magnets with large D   and _vs$v_{\mathrm{s}}$. The dependence of coercivity on D   and _vs$v_{\mathrm{s}}$ can be attributed to the exchange-induced magnetization reversal near the grain boundaries and the low nucleation field of soft phase, respectively. For the anisotropic nanocomposites, the reduced remanence _mr$m_{\mathrm{r}}$ is equal to 1.0$1.0$ for the magnets with small D   or with low _vs$v_{\mathrm{s}}$. However, _mr$m_{\mathrm{r}}$ decreases with increasing _vs$v_{\mathrm{s}}$ for the magnet with large D   due to the influence of dipolar interactions. The difference between the calculated coercivity _Hc$H_{\mathrm{c}}$ with and without considering dipolar interaction shows that the dipolar interaction plays a more important role during the magnetization reversal in the soft phase than that in the hard phase. The maximum calculated energy product of the isotropic nanocomposites is only about 40 MGOe due to the conflicting relation between remanence and coercivity, while that of the anisotropic nanocomposites is 112 MGOe. This reminds us that the alignment of hard grain is important to obtain high performance.     

Simple recipe to synthesize single-domain BaFe12O19 with high saturation magnetization

We report a new synthesis route for preparation of single-domain barium hexaferrite (BaFe₁₂O₁₉) particles with high saturation magnetization. Nitric acid, known as a good oxidizer, is used as a mixing medium during the synthesis. It is shown that formation of BaFe₁₂O₁₉ phase starts at 800 °C, which is considerably lower than the typical ceramic process and develops with increasing temperature. Both magnetization measurements and scanning electron microscope micrographs reveal that the particles are single domain up to 1000 °C at which the highest coercive field of 3.6 kOe was obtained. The best saturation magnetization of ≈60 emu/g at 1.5 T was achieved by sintering for 2 h at 1200 °C. Annealing at temperatures higher than 1000 °C increased the saturation magnetization, on the other hand, decreased the coercive field which was due to the formation of multi-domain particles with larger grain sizes. It is shown that the best sintering to obtain fine particles of BaFe₁₂O₁₉ occurs at temperatures 900-1000 °C. Finally, magnetic interactions between the hard BaFe₁₂O₁₉ phase and impurity phases were investigated using the Stoner-Wohlfarth model.     

Experimental determination of ultra-sharp stray field distribution from a magnetic vortex core structure

The fine magnetic stray field from a vortex structure of micron-sized permalloy (Ni₈₀Fe₂₀) elements has been studied by high-resolution magnetic force microscopy. By systematically studying the width of the stray field gradient distribution at different tip-to-sample distances, we show that the half-width at half-maximum (HWHM) of the signal from vortex core can be as narrow as ∼21 nm at a closest tip-to-sample distance of 23 nm, even including the convolution effect of the finite size of the magnetic tip. a weak circular reverse component is found around the center of the magnetic vortex in the measured magnetic force microscope (MFM) signals, which can be attributed to the reverse magnetization around the vortex core. Successive micromagnetic and MFM imaging simulations show good agreements with our experimental results on the width of the stray field distribution.     

Anomalous magnetization processes and non-symmetrical domain wall displacements in L10 FePt particulate films

Anomalous magnetization processes and non-symmetrical domain wall displacements in the minor loop of L1₀ FePt particulate films were investigated by magnetization measurements and in situ magnetic force microscopy. Magnetization (M) decreases dramatically on increasing the magnetic field to ∼3 kOe after which M becomes small and constant in the range of 5–20 kOe as observed in the successive measurement of minor loops. The domain wall displacement is non-symmetrical with respect to the field direction. The anomalous magnetization behavior was attributed to the non-symmetrical domain wall displacement and large magnetic field required for domain wall nucleation. Energy calculations from modeling suggest that non-symmetrical domain wall displacement is caused by the existence of metastable domains in which the domain edges are stuck to the particle boundaries.     

The effect of compound addition Dy2O3 and Sn on the structure and properties of NdFeNbB magnets

NdFeNbB with the additions of Dy₂O₃ and Sn permanent magnets have been attained by means of powder-blending technique, and their magnetic properties, temperature performance and microstructure were studied in this paper. The addition of just 2.0 wt% Dy₂O₃ or 0.3 wt% Sn proved to be very effective in improving the permanent magnetic properties of NdFeNbB magnets. Dy₂O₃ additions result in the increase in the H_ci and temperature dependence due to the increase of T_c, formation of (NdDy)-rich phase and grain refinement of Φ phase. This improvement of the coercivity stability of the magnets from the addition of Sn is attributed to the smoothing effect of the Sn addition at the grain boundaries. The magnetic properties, the temperature dependence and Curie temperature of NdFeNbB with Dy₂O₃ and Sn combined addition were found to be considerably improved. From the X-ray diffraction, SEM-EDAX studies and the thermo-magnetic study, the improved properties due to the solution of Dy and Sn to the Φ phase, the reduced N_eff and the smaller Φ phase.     

Growth temperature dependence of the hysteretic behavior of Ni0.5Zn0.5Fe2O4 thin films

Herein, a discussion of the effect of deposition temperature on the magnetic behavior of Ni_0.5Zn_0.5Fe₂O₄ thin films. The thin films were grown by r.f. sputtering technique on (1 0 0) MgO single-crystal substrates at deposition temperatures ranging between 400 and 800 °C. The grain boundary microstructure was analyzed via atomic force microscopy (AFM). AFM images show that grain size (φ∼70-112 nm) increases with increasing deposition temperature, according to a diffusion growth model. From magneto-optical Kerr effect (MOKE) measurements at room temperature, coercive fields, H_c, between 37and 131 Oe were measured. The coercive field, H_c, as a function of grain size, reaches a maximum value of 131 Oe for φ ∼93 nm, while the relative saturation magnetization exhibits a minimum value at this grain size. The behaviors observed were interpreted as the existence of a critical size for the transition from single- to multi-domain regime. The saturation magnetization (21 emu/g<M_s<60 emu/g) was employed to quantify the critical magnetic intergranular correlation length (L_c≈166 nm), where a single-grain to coupled-grain behavior transition occurs. Experimental hysteresis loops were fitted by the Jiles-Atherton model (JAM). The value of the k-parameter of the JAM fitted by means of this model (k/μ_o∼50 A m²) was correlated to the domain size from the behavior of k, we observed a maximum in the density of defects for the sample with φ∼93 nm.     

Magnetic domain structure in Fe78.8−xCoxCu0.6Nb2.6Si9B9 nanocrystalline alloys studied by Lorentz microscopy

The magnetic domain structures of Fe_78.8−xCo_xCu_0.6Nb_2.6Si₉B₉ (x=0, 20, 40, 60) alloys are investigated by Lorentz microscopy coupled with the focused ion beam method. The specimen prepared using the FIB method is found to have a considerably more uniform thickness compared to that prepared using the ion-milling method. In Fe_38.8Co₄₀Cu_0.6Nb_2.6Si₉B₉ and Fe_18.8Co₆₀Cu_0.6Nb_2.6Si₉B₉ alloys, 180° domain walls extending in the direction of the induced magnetic anisotropy are observed. Analysis with Lorentz microscopy reveals that the width of the magnetic domains decreases with an increase in the cobalt content or the induced magnetic anisotropy K_u, that is, the domain width d is proportional to the induced magnetic anisotropy (K_u)^−1/4. On the other hand, in the in situ Lorentz microscopy observation as a function of temperature, magnetic ripple structures are found to appear in a localized area due to the fluctuation of magnetization vectors from 423 K. It is observed that the induced magnetic anisotropy caused by the applied magnetic field at 803 K is not suppressed by the magnetic ripple structures observed at 423–443 K.     

Hard–soft composite magnets

A thorough micromagnetic analysis of the exchange-spring problem is reported with special emphasis on multilayers constituted by hard–soft exchange-coupled phases. The developed one—dimensional micromagnetic model leads to a complete magnetic phase diagram in terms of layer thicknesses. Both perpendicular and parallel configurations are considered. The phase diagram provides information on the type of demagnetization processes and the critical fields at which nucleation and reversal take place, depending on the intrinsic properties of the chosen soft and hard materials. The model has been applied to a variety of hard magnetic phases (e.g., FePt, CoPt, SmCo and NdFeB), coupled to different soft materials (e.g., Fe, FeCo, FeRh or permalloy) both in the form of bilayers and multilayers. The most significant results will be highlighted.     

Influence of magnetic (Fe) and non-magnetic (Ga) ion doping at Mn-site on the transport and magnetic properties of La0.7Ca0.3MnO3

The modifications in electrical and magnetic properties of polycrystalline bulk La_0.7Ca_0.3Mn_1−xT_xO₃ (T=Fe, Ga) samples at relatively higher doping concentration (x=0.08-0.12) are investigated. All the synthesized, single phase samples were subjected to resistivity measurements in the temperature range 50-300 K. No insulator-metal transition (T_P) was observed for Fe doped samples with x=0.12. For all the other samples the transition temperature decreased with increase in doping concentration. The small polaron hoping energy was found to increase, rather slowly, with increase in doping concentration. The effect on magnetic properties is also prominently observed with respect to doping element and doping concentration. Interestingly, with the increase in doping concentration, the Curie temperature (T_C) and T_P separate out significantly indicating decoupling of electric and magnetic properties. Changes in these properties have been analyzed on the basis of magnetic disorder introduced in the system due to the magnetic and nonmagnetic nature of these ions rather than strong lattice effects which is insignificant due to similar ionic radii of Fe⁺³ and Ga⁺³ when compared to that of Mn⁺³.     

A study of Sm-substituted SrM magnets sintered using hydrothermally synthesised powders

Anisotropic SrM magnets with Sm substitution, which is observed to have the largest beneficial effect both on the coercivity and on the inhibition of grain growth at high temperature among the other elements such as La, Nd and Pr, were investigated. The average grain size of the samples decreases with increasing Sm/Sr ratio. All the magnets with Sm additions exhibit a bigger coercivity and remanence than those of the SrM magnet without Sm and the coercivity of the magnets increases with increasing Sm/Sr ratio. EDX quantitative analysis suggests that the solubility of Sm³⁺ in the SrM-type structure is very small and that the Sm³⁺ preferably goes into SrFeO_3−x, which is probably located around the SrM grain boundaries. The coercivity mechanism of the magnets is nucleation controlled. The formation and the distribution of the SrFeO_3−x phase around the SrM grain boundraies probably provides the inhibition of SrM grain growth, the reduction of the reverse domain nucleation at the grain surface and the isolation of the SrM grains. All these factors would contribute to the improvements of the coercivity of the magnets with Sm additions.     

Li0.5Fe2.5−xMnxO4 ferrite sintered from microwave-induced combustion

Li_0.5Fe_2.5−xMn_xO₄ (0≦x≦1.0) powders with small and uniformly sized particles were successfully synthesized by microwave-induced combustion, using lithium nitrate, ferric nitrate, manganese nitrate and carbohydrazide as the starting materials. The process takes only a few minutes to obtain as-received Mn-substituted lithium ferrite powders. The resultant powders annealed at 650 ^°C for 2 h and were investigated by thermogravimeter/differential thermal analyzer (TG/DTA), X-ray diffractometer (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), and thermomagnetic analysis (TMA). The results revealed that the Mn content were strongly influenced the magnetic properties and Curie temperature of Mn-substituted lithium ferrite powder. As for sintered Li_0.5Fe_2.5−xMn_xO₄ specimens, substituting an appropriate amount of Mn for Fe in the Li_0.5Fe_2.5−xMn_xO₄ specimens markedly improved the complex permeability and loss tangent.     

Extracting domain wall patterns from SEM magnetic contrast images

The magnetic contrast images of a soft magnetic metallic glass Fe₇₉Si₆B₁₄Cu₁ subjected to a periodic magnetic field were recorded with a scanning electron microscope by using a stroboscopic technique. An image processing method for the extraction of domain patterns from these images is presented. By this technique, delicate details of the dynamic magnetization process can be investigated and differences in the local magnetisation and domain wall movement can be analysed.