Crystallization and magnetic properties of melt-spun two-phase nanocrystalline Nd-Fe-B alloy

A new type of permanent magnet alloy with composition Nd_9.32Fe_85.32B_5.36 has been prepared by a melt spinning method. After optimized annealing of the initial amorphous alloy, high magnetic properties are obtained in the isotropic specimens. Remanence, energy product and intrinsic coercivity are 1.09 T, 153.6 kJ m⁻³ and 400 kA m⁻¹, respectively. The samples consist of two phases, a matrix of nanometer-sized hard magnetic Nd₂Fe₁₄B phase (about 40 nm) together with numerous -iron particles (about 20 nm) embedded in it. The crystallization behavior for amorphous samples has been studied. The results indicate that the -iron initially precipitates from the amorphous matrix, and at higher annealing temperatures the crystallization of the Nd₂Fe₁₄B phase occurs. No metastable phase was observed in all heat treatments. Although the volume fraction of the magnetically soft -iron is about 30 vol%, the second quadrant of the J-H loop is typical of a magnetically soft hard material. The role of exchange coupling between the magnetically soft grain and the magnetically hard grain is discussed.     

Synthesis, stability against air and moisture corrosion, andmagnetic properties of finely divided looseNd2Fe14BHx, x⩽5, hydride powders

Nd₂Fe₁₄BH_x, x⩽5, hydride powders, with particle size as small as 1 μm, have been successfully prepared using a chemical method derived from the well-known oxide-reduction diffusion (ORD) method. In this method, the raw materials (Nd₂O₃, iron and boron) are mixed with calcium metal or hydride powder (in excess) and additions of anhydrous CaCl₂ and NaCl, and finally sintered at 1170-1270 K for a few hours under an argon atmosphere. This yields finely divided Nd₂ Fe₁₄B crystallites embedded in the byproducts. The material is then washed with water at room temperature, where the excess Ca in the mixture reacts with water and produces nascent hydrogen, which reacts with the alloy particles embedded in the byproducts, and finally yields a well-separated Nd₂Fe₁₄BH_x, x⩽5, hydride powder. Thermal stability, crystalline structure, and magnetic properties of several hydrided powders are studied systematically. These studies show that the interstitial hydrogen atoms led to 1) an increase in the lattice volume by as much as 4.2%, 2) a decrease in the coercivity to almost zero, 3) a dramatic improvement in T_C from 593 to 642 K, and 4) a substantial modification of the magnetization process, showing magnetic saturation at lower fields of ≈60 kOe (against ≈150 kOe in anhydride)     

Design and performance of a permanent-magnet rotary refrigerator

In order to demonstrate the potential of magnetic refrigeration to provide useful cooling near room temperature, Astronautics Corporation of America constructed a rotary magnetic refrigerator (RMR) in 2001. The RMR uses the active magnetic regenerator (AMR) cycle with an aqueous heat transfer fluid. The required change in magnetic field is produced by the rotation of a wheel packed with porous beds of magnetocaloric material through a 1.5 T Nd₂Fe₁₄B permanent magnet with steel flux concentration poles. A pump, and valves mounted to the wheel, control heat transfer fluid flow through the magnetocaloric beds and heat exchangers. This rotary design allows quiet, reliable operation over a range of frequencies (0.5–4 Hz), heat transfer fluid flow rates and cooling power. The performance of the device using Gd and Gd alloy spherical particles is reported and analyzed. We also describe the performance effects of introducing layered beds and an La(Fe_1−xSi_x)₁₃H_y alloy with a first order magnetic transition.     

Coercivity and spin reorientation transitions in Nd-Fe-Bnanocomposites prepared by melt spinning

Alloys of composition Nd₉Fe₈₅B₆, Nd_11.76Fe_82.46B_5.88, and Nd₁₈Fe₇₆B₆ were prepared by melt spinning at roll velocities from 19 to 25 m/s. The grain size distribution of rapidly quenched flakes was evaluated by means of X-ray diffraction line broadening. The average grain size of rapidly quenched Nd-Fe-B alloys is within a range from 19 to 40 nanometers and differs from the roll contact side to the free side of the flakes. For the first time, the spin reorientation transitions T_ST of nanophase Nd ₂Fe₁₄B alloys have been determined. They were found to be lower than that of bulk Nd₂Fe₁₄B. The smaller the grain size, the lower is T_ST. Also for the first time, the temperature dependence of the coercivity of nanophase Nd-Fe-B magnets was determined from 4.2 to 300 K by measuring hysteresis loops on a single flake in a pulsed-field magnetometer with a field strength up to 24 MA/m. The coercivity of the nanophase Nd-Fe-B has less of a temperature dependence than sintered magnets     

Magnetic properties of melt spun NdFe10Cr2-Nd0.67B0.33 pseudobinary alloys

The coercivity of the melt-spun pseudobinary (NdFe₁₀Cr ₂)_1-x (Nd₂B)_x alloys, in which Nd₂B represents a composition of Nd_0.67B_0.33, was systematically studied. It was found that significant coercivities are possible with optimal additions of the Nd-B composition at x=0.5-0.7. The as-spun (substrate velocity=10 m/s) coercivity increased from 0.1 kOe at x=0.0 to maxima of 7.0 and 7.5 kOe at x=0.5 and 0.7, due to the Nd₂ Fe₁₄B and a new Fe-Nd phase, respectively, as evidenced from thermomagnetic analysis and X-ray diffraction. Annealing the overquenched amorphous x=0.7 alloy led to the crystallization of the Nd₂Fe₁₄B phase, and a coercivity of 8.5 kOe was obtained     

A Nd-Fe-O intergranular phase in Nd-Fe-B sintered magnets and itseffect on coercivity

The intergranular microstructure and coercivity of Nd richer Nd _xFe_93-xB₇ (x=16-28) sintered magnets have been systematically studied by means of scanning electron microscopy, analytical transmission electron microscopy, scanning Auger multiprobe, thermomagnetic analysis, magnetic measurement and annealing experiments. A new stable Nd-Fe-O ferromagnetic phase with a composition NdFe₂O_x (x≈0.3) and a Curie temperature of 145°C is found in the intergranular regions of the magnets, due to the introduction of a considerable amount of oxygen during magnet processing and its segregation in the intergranular regions. The phase forms at ~650°C and volume fraction reaches a maximum of ~4% in the Nd₂₂Fe₇₁B₇ magnets. This new phase has a strong hindrance effect on the propagation of reversed domain walls between Nd₂Fe₁₄B grains, and thus leads to a considerable enhancement of coercivity. Raising the Curie temperature of this phase would be a new important approach to improve the high-temperature coercivity of Nd-Fe-B magnets     

Magnetic Domain Imaging of Nd2Fe14B Single Crystals With Unmodified Scanning Electron Microscopy

The stray flux manifestations of surface magnetic domains found in as-grown Nd₂Fe₁₄B single crystals were observed by conventional scanning electron microscopy (SEM) without instrumental modifications. Kerr optical microscopy was employed to confirm the results obtained by SEM. Spike domains were observed on the (001) plane, while a lozenge-type domain pattern was observed on (223) plane of Nd₂Fe₁₄B. A modified image-distortion mode was applied to image the three-dimensional stray flux emanating from the sample. The optimum scanning electron microscope imaging conditions are attained with an incident-electron energy set at 5 to 6kV, which produced images with resolution on the order of 1μm. The simplicity of the technique and the ready adaptability of the SEM to such modifications as in situ current and magnetic field application suggest the extension of these to investigations of other materials of technological interest, such as perpendicular media disks.     

Magnetic behaviour of Cd and Cr substituted cobalt ferrites

Polycrystalline samples with general formula Cd_xCo_1−xFe_2−yCr_yO₄ (x=0, 0.25, 0.50, 0.75 and 1.00; y=0, 0.15 and 0.30) were prepared by standard ceramic techniques. The samples were characterized by XRD, IR, SEM and VSM techniques. The magnetic properties were studied at room temperature. The Neel's two-sublattice model is found to exist for lower concentration of Cd (x<0.25). Thereafter (x≥0.25) the canted spin model is found to exist for which Yafet–Kittel (Y–K) angles are calculated. The saturation magnetic moment is found to reduce with the substitution of Cr³⁺, and is explained on the basis of cation distribution. No magnetic transformation is observed for the samples with higher cadmium concentrations (for x=0.75 and 1.00).     

Magnetic Properties of Y3Fe5O12 Nanoparticles Doped Bi and Ce Ions

Y_2.9-xCe_0.1Bi_xFe₅O₁₂ (x = 0-0.5) nanoparticles ranging from 58 to 63 nm were fabricated by a sol-gel method, and their crystallite structures and magnetic properties were investigated by X-ray diffraction (XRD), IR spectroscopy, and vibrating sample magnetometer (VSM). Results of VSM show that the saturation magnetization intensity increased with increase in Ce content (0.1), decrease in Bi concentration (x), and increase in particle size of the formulation.     

Effect of Chromium on Magnetic Properties of Y2.9Ce0.1Fe5-xCrxO12 Nanoparticles

Y_2.9Ce_0.1Fe_5-xCr_xO₁₂ (x = 0-0.5) nanoparticles were fabricated by a sol-gel method. Samples with particle size ranging from 60 to 64 nm were obtained and their crystalline structures and magnetic properties were investigated by X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). Results of VSM show that the saturation magnetization is increased firstly, after decreased with the Cr concentration (x). The saturation magnetization is increased with increasing the particle size.     

Consolidation of Sm5Fe17 powder by spark plasma sintering method

Sm₅Fe₁₇ bulk materials, one of the newer permanent magnetic materials, were successfully produced by the spark plasma sintering method. The resultant bulk materials had high densities of 85–98%. When obtained by sintering at relatively lower temperatures, the Sm₅Fe₁₇ bulk materials consisted of the Sm₅Fe₁₇ and SmFe₃ phases, whereas they contained some -Fe phase together with the Sm₅Fe₁₇ and SmFe₃ phases when obtained by sintering at relatively high temperatures. High coercivity values, exceeding 2 MAm⁻¹, were found in the Sm₅Fe₁₇ bulk materials consisting of the Sm₅Fe₁₇ and SmFe₃ phases.     

Influence of wheel speed during planar flow melt spinning on the microstructure and soft magnetic properties of Fe<Subscript>68.5</Subscript>Si<Subscript>18.5</Subscript>B<Subscript>9</Subscript>Nb<Subscript>3</Subscript>Cu<Subscript>1</Subscript> ribbons

The structure and soft magnetic properties of Fe_68.5Si_18.5B₉Nb₃Cu₁ (at.%) alloy ribbons produced through planar flow melt spinning at different wheel speeds viz. 34, 17 and 12 m/s have been investigated using X-ray diffraction, differential scanning calorimetry, transmission electron microscopy, vibrating sample magnetometer and positron lifetime spectroscopy. Amorphous ribbons formed with different wheel speeds manifested different enthalpy and activation energy of crystallization. The volume fraction of nanocrystalline phase, saturation magnetization and permeability are found to increase whereas coercivity is found to decrease with increasing wheel speed on annealing. A detailed analysis of positron lifetime spectra obtained from the as-spun ribbons has been used to rationalize the variation in microstructure and magnetic properties. The presence of larger number of defects at higher wheel speed increases the volume fraction of nanocrystalline phase on annealing which improves the soft magnetic properties.     

Influence of thermal treatments on the elastic parameters in iron rich metallic glasses

The change of magnetoelastic properties after thermal treatments has been investigated for two groups of metallic glasses. (Fe₇₉Co₂₁)_75+xSi_15−1.4xB_10+0.4x (x (at.%)=0, 2, 4, 6, 8, 10) has been studied both in the as-prepared state and after thermal annealing in an applied magnetic field, to achieve a particular domain structure, at temperatures well below the crystallization temperatures. Changes in the ΔE effect, magnetomechanical coupling (k) and internal friction coefficient (Q⁻¹) are reported, reaching values of about 60% of the saturation value E_S. Fe₆₄Ni₁₀Nb₃Cu₁Si₁₃B₉ alloys annealed in vacuum for 1 h in the temperature range 350–550 °C showed maximum values of the ΔE effect and k of 61% and 0.85, respectively, accompanied by a minimum value of Q of around 2 for the sample annealed at 460 °C. These variations are related to the progress of nanocrystalization. The properties achieved are among the best reported for magnetomechanical applications.     

Mechanical characterization of Ni1−xZnxFe2O4 prepared by non-conventional methods

The mechanical properties like hardness, H_v and compressive strength, σ of Ni_1−xZn_xFe₂O₄ (x = 0.2, 0.3, 0.4 and 0.5) prepared by the non-conventional flash combustion and citrate-gel decomposition techniques are studied and reported. It is observed that there is an increase in hardness with zinc content as well as sintering temperature. The hardness in the order of 2.0–3.63 GPa and compressive strength in the order of 150–240 MPa are obtained for Ni–Zn ferrites prepared by these non-conventional techniques. The influence of density, porosity and microstructure on hardness and compressive strength of Ni–Zn ferrites with respect to sintering temperature was studied.     

Effect of deposition temperature on the structural and thermoelectric properties of bismuth telluride thin films grown by co-sputtering

Thermoelectric bismuth telluride thin films were prepared on SiO₂/Si substrates by radio-frequency (RF) magnetron sputtering. Co-sputtering method with Bi and Te targets was adopted to control films' composition. Bi_xTe_y thin films were elaborated at various deposition temperatures with fixed RF powers, which yielded the stoichiometric Bi₂Te₃ film deposition without intentional substrate heating. The effects of deposition temperature on surface morphology, crystallinity and electrical transport properties were investigated. Hexagonal crystallites were clearly visible at the surface of films deposited above 290 °C. Change of dominant phase from rhombohedral Bi₂Te₃ to hexagonal BiTe was confirmed with X-ray diffraction analyses. Seebeck coefficients of all samples have negative value, indicating the prepared Bi_xTe_y films are n-type conduction. Optimum of Seebeck coefficient and power factor were obtained at the deposition temperature of 225 °C (about − 55 μV/K and 3 × 10^− 4 W/K²·m, respectively). Deterioration of thermoelectric properties at higher temperature could be explained with Te deficiency and resultant BiTe phase evolution due to the evaporation of Te elements from the film surface.     

SPS界面反应增强机制调控的软磁复合材料磁性能和电阻率

设计软磁复合材料(SMCs)的绝缘层要兼顾软磁性能和电阻率。本研究以Fe/Ni_0.5Zn_0.5Fe₂O₄复合体系为例, 研究界面MnO₂氧化剂对样品软磁性能和电阻率的影响, 揭示提高软磁性能和电阻率的SMCs界面放电等离子烧结(SPS)氧化还原机制。采用球磨法制备添加0、0.1wt%、0.3wt%、0.5wt%和1.0wt% MnO₂的核壳结构Fe@Ni_0.5Zn_0.5Fe₂O₄(MnO₂)复合粉末, 随后SPS烧结制备Fe/Ni_0.5Zn_0.5Fe₂O₄(MnO₂)块体SMCs样品, 通过扫描电镜(SEM)、X射线衍射(XRD)表征该样品的结构特征, 用精密电阻测试仪和振动样品磁强计测试该样品的电阻率和磁性能。研究发现, 添加0.5wt% MnO₂的Fe/Ni_0.5Zn_0.5Fe₂O₄(MnO₂)块体SMCs样品比未添加样品电阻率提高33.7%、饱和磁化强度提高6.9%。研究结果表明, SPS烧结增强SMCs界面快速氧化还原反应, MnO₂氧化剂的添加使界面铁氧体离子浓度变化, 降低了B位电子跃迁频率, 提高有效波尔磁子数及B-B磁超交换作用, 表现出同时提高SMCs的软磁性能和电阻率的多重效应。     

复合磁性催化剂β-MnO2/MnxZn1-xFe2O4的制备与表征

采用化学共沉淀法制备了以Mn_xZn_1-x Fe₂O₄为磁性基体的β-MnO₂/Mn_xZn_1-xFe₂O₄复合磁性催化剂,利用XRD、SEM、FTIR和超导量子干涉仪对复合磁性催化剂的结构和性能进行了表征,以罗丹明B （RhB）为模拟污染物,研究了β-MnO₂/Mn_xZn_1-xFe₂O₄的催化活性,并考察了其稳定性。结果表明,球状的β-MnO₂与块状的磁性基体Mn_xZn_1-xFe₂O₄成功复合,且制备的β-MnO₂/Mn_xZn_1-xFe₂O₄复合磁性催化剂具有良好的催化性能和磁学性能。当Mn_xZn_1-xFe₂O₄与β-MnO₂的质量比为20：100时,在2 mL含量为30%的H₂O₂作用下,1 h内β-MnO₂/Mn_xZn_1-xFe₂O₄复合磁性催化剂对100 mL浓度为10 mg/L的RhB降解率（93.9%）远高于纯β-MnO₂（33.7%）;在磁场作用下,β-MnO₂/Mn_xZn_1-xFe₂O₄复合磁性催化剂的回收率为89%,经过5次循环利用之后其对RhB的降解率仍达76%。     

Fe3O4磁性导体表面磁控溅射NdCoCr薄膜组织和磁性分析

采用磁控溅射工艺,以Fe₃O₄磁性导体作为基底材料在其表面制得Nd Co Cr合金薄膜,分析了加入不同比例Co的情况下制得的Nd-Co非晶薄膜垂直磁各向异性(PMA)性能及其磁畴特征,同时对退火态薄膜组织相成分和磁性进行研究。结果表明:本实验制得了具有非晶形态的薄膜结构,当薄膜内的Co含量增加后,形成了强度更高的Fe₃O₄衍射峰。当Co含量逐渐增大后,M_s发生了不断增强。初始薄膜K_eff表现为随Co含量增大而提高。Co含量为4%试样MFM图像上形成了明暗相间条纹。通过MFM方法测试得到的ΔΦr曲线表现为与Ku曲线形状具有明显相似性,都在Co含量为6%位置处达到最大值。各退火态试样中都形成了Nd₄Co₃、Nd₂Co₁₇、Nd Co Cr₂。当薄膜内析出Nd Co Cr₅与Nd₂Co₇纳米晶后,获得了更大矫顽力,当Co含量大于4%时,退火态薄膜形成了较低的矫顽力。     

PrBi4Fe0.5Co0.5Ti3O15多铁陶瓷的性能研究

采用传统固相反应法与两步合成法制备了PrBi₄Fe_0.5Co_0.5Ti₃O₁₅陶瓷, 研究了Pr与Co共掺杂对Bi₅FeTi₃O₁₅陶瓷的结构、磁性能以及介电性能的影响。X射线衍射分析显示, 传统固相反应法制备的样品比两步法制备的样品更容易形成单相结构。铁电和磁性测量证明样品具有多铁性, 并且Pr与Co共掺杂能大幅提高材料的磁性能, 固相反应法与两步合成法制备的样品在室温下的剩余磁化强度(2M_r)分别为0.315, 0.576 Am²/kg, 比文献报道的Bi₅FeTi₃O₁₅陶瓷的2M_r ( 2.7 Am²/kg ) 高5个数量级, 比掺Co的Bi₅Fe_0.5Co_0.5Ti₃O₁₅陶瓷2M_r ( 7.8×10^-3 Am²/kg ) 高2个数量级。     

EPR and SQUID studies on magnetic properties of SiO2-doped Ni–Zn ferrite nanocomposites

Effects of the silica content and temperature on the magnetic properties of Ni_0.5Zn_0.5Fe₂O₄/SiO₂ nanocomposites have been studied by electron paramagnetic resonance (EPR) and superconducting quantum interference device (SQUID) technique. The content of TEOS in the starting solution affects the interaction between NiZn ferrite and silica, and then determines the particle size and the EPR properties. In addition, the SQUID properties of the composites were sensitive to particle size. It was observed that the saturation magnetization (M_s), remnant magnetization (M_r) and initial susceptibility (χ_i) decreased with increasing SiO₂ content.