Electromagnetic wave-absorption properties of rapidly quenched of Nd–Fe–B nanocomposites with low Nd content

The electromagnetic wave-absorption properties of Nd₃Fe_68−xMn_xCo₁₈B₁₁ (x=0, 1, 2) alloys obtained by rapid quenching from the melt was studied. The complex permittivity-frequency and permeability-frequency properties were determined in the microwave frequency regime of 2–18 GHz by vector network analysis. XRD spectra showed that only α-Fe diffraction peak was observed in the as-spun alloys. It is found that the acquired complex permittivity and permeability values match the microwave frequency when the 1 at% Mn content was doped. A minimum reflection loss of −6.9 dB is obtained at 2.7 GHz for composite Nd₃Fe₆₆Mn₂Co₁₈B₁₁ with absorber thickness of 1.5 mm. The exchange interaction was attributed to the microwave absorption properties. The results suggest a new design of microwave absorbers based on electromagnetic wave-absorbing materials.     

Unusual magnetization anisotropy in amorphous Nd–Fe–Al ribbons

Nd₆₀Fe₃₀Al₁₀ ribbons has been prepared by chill-block melt-spinning with different wheel speeds from 5 to 30 m/s. Fully amorphous ribbons were obtained at wheel speeds of 25 and 30 m/s. These ribbons exhibited an unusually large anisotropy in magnetization. The effect of the magnetic anisotropy decreased with decreasing wheel speed, and nearly disappeared at the wheel speed of 5 m/s, at which the ribbon consisted of a mixture of a more stable Fe-rich amorphous phase and a crystalline Nd phase with a strong crystallographic texture.     

Effects of post-sinter annealing on microstructure and magnetic properties of Nd–Fe–B sintered magnets with Nd–Ga intergranular addition

We investigate the effects of post-sinter annealing on the microstructure and magnetic properties in B-lean Nd–Fe–B sintered magnets with different quantities of Nd–Ga intergranular additions. The magnet with fewer Nd–Ga additions can enhance 0.2 T in coercivity, with its remanences nearly unchanged after annealing. With the further increase of the Nd–Ga addition, the annealing process leads coercivity to increase 0.4 T, accompanied by a slight decrease of remanence. With the Nd–Ga addition further increasing and after annealing, however, the increase of coercivity is basically constant and the change of remanence is reduced. Microstructure observation indicates that the matrix grains are covered by continuous thin grain boundary phase in the magnets with an appropriate Nd–Ga concentration after the annealing process. However, the exceeding Nd–Ga addition brings out notable segregation of grain boundary phase, and prior formation of part RE6 Fe13 Ga phase in the sintered magnet. This prior formation results in a weaker change of remanence after the annealing process.Therefore, the diverse changes of magnetic properties with different Nd–Ga concentrations are based on the respective evolution of grain boundary after the annealing process.     

Progress in recycling of Nd–Fe–B sintered magnet wastes

Significant efforts have been put into the recycling of bulk Nd–Fe–B sintered magnet wastes around the world in the past decade because bulk Nd–Fe–B sintered magnet wastes are valuable secondary rare-earth resources.There are two major facts behind the efforts.First, the waste magnets contain total rare-earth content as high as more than 30 wt.%, which is higher than most natural rare-earth mines.Second, the waste magnets maintain the physical and chemical properties of the original magnets even with deterioration of the properties on surfaces due to corrosion and contamination.In this review,various techniques for recycling bulk Nd–Fe–B sintered magnet wastes, the overall properties of the recycled Nd–Fe–B sintered magnets, and the mass production of recycled magnets from the wastes are reviewed.     

Coercivity mechanism of La–Nd–Fe–B films with Y spacer layer

The effect of the Y spacer layer on the phase composition, coercivity, and magnetization reversal processes of La–Nd–Fe–B films has been investigated. The addition of a 10 nm Y spacer layer increases the coercivity of the film to 1.36 T at 300 K and remains 0.938 T at 380 K. As the thickness of the Y spacer layer increases, Y participates in the formation of the main phase in the film, and further regulates the formation of La–B phases. The results of the first-order reversal curve(FORC) and mic...     

Investigation on bulk Nd–Fe–Al amorphous/nano-crystalline alloy

Cylindrical ingots of bulk amorphous Nd₇₀Fe₂₀Al₁₀ with a diameter of 8 mm were prepared by a copper mold casting method. It was proved experimentally with X-ray diffraction, scanning electron microscopy and differential scanning calorimetry that the as-prepared alloy samples consisted mainly of the amorphous phase with a minute amount of nano-crystalline phase. The onset crystallization temperature (T_x) and the melting temperature (T_m) of the samples were 743 and 823 K, respectively, from DSC results. The temperature interval between T_x and T_m, ΔT=T_m−T_x, is 80 K and the resulting ratio of T_x/T_m is 0.90. Both a high T_x/T_m ratio and a small ΔT are considered the reasons for the good glass-forming ability. The Curie temperature (T_c) of these samples was 525 K from magneto-thermal gravimetric analysis. This measured value is higher than the highest T_c among binary Nd–Fe amorphous alloys. Annealing treatments were carried out for the as-cast samples to obtain dual-phase samples with different volume fractions of nano-crystalline phase. Magnetic measurement results indicated that the hard magnetic behavior is weakest for samples with 40% of nano-crystalline phase. The curve of the measured hysteresis loop area versus the volume fraction of nano-crystalline phase concaves upward, which agrees with what we predicated in our previous simulation results.     

Formation and crystallization kinetics of Nd–Fe–B-based bulk amorphous alloy

In order to improve the glass-forming ability (GFA) of Nd–Fe–B ternary alloys to obtain fully amorphous bulk Nd–Fe–B-based alloy, the effects of Mo and Y doping on GFA of the alloys were investigated. It was found that the substitution of Mo for Fe and Y for Nd enhanced the GFA of the Nd–Y–Fe–Mo–B alloys. It was also revealed that the GFA of the samples was optimized by 4 at.% Mo doping and increased with the Y content. The fully amorphous structures were all formed in the Nd $_{6-{x}}$ Y $_{{x}}$ Fe $_{68}$ Mo $_{4}$ B $_{22}$ (x $=$ 1–5) alloy rods with 1.5 mm-diameter. After subsequent crystallization, the devitrified Nd $_{3}$ Y $_{3}$ Fe $_{68}$ Mo $_{4}$ B $_{22}$ alloy rod exhibited a uniform distribution of grains with a coercivity of 364.1 kA/m. The crystallization behavior of Nd $_{3}$ Y $_{3}$ Fe $_{68}$ Mo $_{4}$ B $_{22}$ BMG was investigated in isothermal situation. The Avrami exponent n determined by JAM plot is lower than 2.5, implying that the crystallization is mainly governed by a growth of particles with decreasing nucleation rate.     

Synthesis and Stabilization of Fe–Nd–B Nanoparticles for Biomedical Applications

Stable composition of Iron Neodymium Boron nanoparticles are formed by a chemical method. Conventional borohydride reduction method was used. The particles are in the size range of 30–100 nm. Silica coating was applied to stabilize and prepare the particles for in vitro applications such as cell separation and diagnostics. Morphology of particles has been studied along with the structure and magnetic properties.     

Effects of oxidation of DyH_3 in Nd–Fe–B sintered magnets

The effects of oxidation of Dy H3 with respect to dysprosium addition to Nd–Fe–B sintered magnets are examined.Samples sintered with the addition of freshly milled dysprosium hydride, dysprosium hydride exposed to air at room temperature for 15 min and dysprosium hydride exposed to air at 100°C for 3.5 hours are studied from the aspects of magnetic properties, microstructures, and their degradation, respectively. It is found that some oxidized dysprosium is distributed in the Nd-rich phase; hence, the decrease of remanence occurred. The degradation results indicate that preoxidised dysprosium can be a major factor in increasing the corrosion rate. The microstructures and corrosion acceleration test suggested that the oxidation is detrimental to remanence.     

Ultra-fine grained Nd–Fe–B by high pressure reactive milling and desorption

This paper reports on the grain refinement in dynamic hydrogenation disproportionation desorption and recombination (d-HDDR) processed Nd-rich Nd₂Fe₁₄B and stoichiometric Nd₂Fe₁₄B powders using high pressure reactive milling (HPRM) followed by a subsequent desorption and recombination. In contrast to the dynamic-HDDR processed anisotropic powder with a grain size of the Nd₂Fe₁₄B phase of 300 nm, the new approach yields a further reduction of the Nd₂Fe₁₄B₁ grain size to less than 70 nm. Nd-rich Nd₂Fe₁₄B powder produced by HPRM and subsequent desorption exhibits a coercivity μ_0iH_c=1.35 T and a remanence of 0.80 T. In the stoichiometric material, the reduction of the Nd-content leads to an increase in remanence to 0.85 T. Additionally, it is demonstrated that highly anisotropic powders can also be obtained by dynamic-HDDR processing of stoichiometric Nd₂Fe₁₄B powders.     

Hyperfine Field and Isomer Shift Evolution in Hydrogenated Nd–Fe–B Alloy

RE₂Fe₁₄B (RE=rare earth) materials are capable of absorbing hydrogen to form a stable solid solution at room temperature. Hydrogenation produces a number of significant changes in the hyperfine interactions. In this work, ⁵⁷Fe Mössbauer effect spectroscopy and X-ray diffraction measurements were performed on Nd_14.01Hf_0.08Fe_78.91B_7.00 alloys submitted to thermal treatment in hydrogen atmosphere. A non-linear increase of the hyperfine fields and isomer shifts with hydrogen concentration was observed. The hyperfine parameters of the 8j₁ site exhibit a rather different evolution than those experienced by the other major sites (8j₂, 16k₁, 16k₂). The origin of the hyperfine field enhancement is analyzed in terms of volume expansion and H nearest neighbors to the Fe sites. A linear expression on these two effects to give account of isomer shift evolution for 8j₁ site is given.     

Understanding the high temperature oxidation and ignition behaviour of two-phase Mg–Nd alloys and a comparison to single phase Mg–Nd

The oxidation kinetics and the mechanism of two-phase Mg–Nd alloys were investigated via isothermal heating experiments conducted in dry air at 500 °C for 12 h. The oxidation kinetic curves reveal improved oxidation resistance on neodymium (Nd)-containing alloys compared to pure Mg. A lower mass gain was detected at 2.5-%Nd than at 6-Nd%, which was related to the lower amount of intermetallic phase on the alloy surface. The intermetallic phase has a significant effect on the oxide growth stage. Nd₂O₃ formation on the intermetallic phases creates diffusion paths for oxygen to the metal/oxide interface, affecting both the oxidation kinetics and the oxidation resistance of the alloys. The formation of a Nd-depleted region at the subsurface due to extensive Nd oxidation at the oxide/intermetallic interface lowers the protective ability of the oxide scale. As increasing the Nd content of binary Mg–Nd alloys above 0.5 wt% shifts the alloys from single-phase region to two-phase region, it adversely affects the ignition resistance.     

Plastic deformation modeling of backward extrusion process for Nd–Fe–B ring magnets

3D finite element-based software (3D DEFORM) was used to simulate the thermal extrusion process of nanocrystalline magnetic ring. The effective stresses and effective strains for a ring magnet at different stages of the extrusion process were determined by simulation. The effective strains at different stages are displayed. The effective stresses on the cross section are determined by simulation. The test results of magnetic properties were of good validation of the three-dimensional finite element analysis for nanocrystalline backward extruded ring. 3D finite element-based plastic deformation simulation is proved to be an effective way to analyze the hot extrusion process of nanocrystalline magnetic ring, and to provide guiding for the mold design of thermal extrusion.     

Coercivity enhancement of anisotropic Dy-free Nd–Fe–B powders by conventional HDDR process

Coercivity enhancement of Dy-free Nd–Fe–Co–B–Ga–Zr powders was studied using the conventional hydrogenation–decomposition–desorption–recombination (HDDR) process. It was found that the addition of Al together with the proper Nd content and the slow hydrogen desorption of the HDDR treatment can induce high coercivity in the powder. For example, the 14.0 at% Nd–2.0 at% Al powder exhibits H_cJ of 1560 kA/m, B_r of 1.22 T, and (BH)_max of 257 kJ/m³. The high coercivity inducement of the powder is thought to be attributed to the formation of Nd-rich phase, which continuously surrounds fine Nd₂Fe₁₄B grains.     

Regulating element distribution to improve magnetic properties of sintered Nd–Fe–B/Tb–Fe–B composite magnets

Nd content was varied in Nd_(13.2-x)Fe_(80.8+x)B_6(x = 0, 0.5, 1, and 1.5) to optimize the magnetic properties of sintered Nd–Fe–B/Tb–Fe–B composite magnets, which were prepared by mixing 9 g of Nd–Fe–B with 1 g of Tb_(17)Fe_(75)B_8 powder.In conventional magnets, by reducing Nd content, the coercivity of 10.4 kOe in Nd_(13.2)Fe_(80.8)B_6 decreases to 7.2 kOe in Nd_(12.2)Fe_(81.8)B_6; meanwhile, in Nd–Fe–B/Tb–Fe–B magnets the coercivity does not decrease when reducing Nd content.In the intergranular phase, the Tb content increases owing to the reducing Nd content of the Nd–Fe–B alloy in the sintered composite magnets.Therefore, the excess Tb in Tb_(17)Fe_(75)B_8 enters the intergranular phase, and more Tb atoms can substitute for Nd at the grain boundary of the Nd–Fe–B phase, leading to a more significant increase in coercivity.The remanence increases with reducing Nd content, and the energy product of 39.1 MGOe with a high coercivity of 21.0 kOe is obtained in Nd_(12.2)Fe_(81.8)B_6/Tb_(17)Fe_(75)B_8 magnets.These investigations show that magnetic properties can be further improved by regulating the element distribution in sintered composite magnets.     

Magnetic domain structures of overquenched Nd–Fe–B permanent magnets studied by electron holography

Microstructures and magnetic domain structures of overquenched Nd–Fe–B permanent magnets have been investigated in detail by transmission electron microscopy. While magnetic domain boundaries are clarified by Lorentz microscopy, magnetization distribution in the domains is clearly observed by electron holography. In the as-quenched magnet, the size of the magnetic domains is in the range from 200 to 500 nm and the direction of the magnetic lines of force changes gradually in wide region, while in the annealed one having the crystalline phase of Nd₂Fe₁₄B, the direction of the magnetic lines of force changes drastically especially at the grain boundaries. Furthermore, the direction of the magnetic lines of force changes more drastically in the specimen annealed at 893 K than the specimen annealed at 843 K. This result clearly indicates that the magnetocrystalline anisotropy is enhanced with the increase of annealing temperature, resulting in strong domain wall pinning.     

A study of nanostructure magnetosolid Nd–Ho–Fe–Co–B materials via atomic force microscopy and magnetic force microscopy

Nanostructure Nd–Ho–Fe–Co–B alloys have been probed via atomic force microscopy and magnetic force microscopy (AFM and MFM, respectively). The ribbon samples with a thickness of ~30 μm are prepared via the rapid solidification on a rotating copper barrel. A part of samples has been subjected to hydration, whereas another one has undergone severe plastic deformation. AFM was mainly used to study the contact and free surface of ribbon samples. This has enabled us to establish the topography, structure, defects of both sides, morphology of magnetic inclusions of the initial quenched samples and the materials subjected to the subsequent external effects. The AFM and MFM data allowed the magnetic hysteresis properties of the bulk samples with the identical composition to be interpreted.     

Effect of very small additions on the coercivity of Dy-free Nd–Fe–(Co)–B-sintered magnets

The effect of small substitutions on the coercivity of Nd–Fe–B and Nd–Fe–Co–B-sintered magnets has been investigated. Addition of 0.18 at% Ga was found to be the most effective for improving the coercivity in both Nd–Fe–B and Nd–Fe–Co–B without decreasing much the remanent magnetization. Scanning electron microscopy on Ga-free and Ga-added magnets did not reveal a noticeable difference in phase morphology. However, Fe and especially Co concentrations in the intergranular Nd-rich phase were found to be markedly increased after the small Ga addition. Combined addition of Co with a small amount of Cu did not increase the coercivity of the Dy-free magnets. However, none of the examined very small additives can yet be considered as an alternative to Dy for extending operating temperature range of the high-energy Nd–Fe–B magnets.