Effect of additions of zinc stearate on the properties of sintered Nd-Fe-B magnets

Zinc stearate additions have been used to increase the remanence of sintered Nd-Fe-B magnets produced by the powder metallurgy without powder pressing. Zinc stearate acts as an internal lubricant, i.e., it decreases the friction forces between the particles and favors an increase in the degree of texture of the powders, which is induced by the magnetic field. It is shown that the density and the magnetic hysteresis characteristics of sintered magnets produced using additions of 0.15 wt % zinc stearate exceeds the corresponding values obtained for magnets produced without this addition at a filling density of powders in containers of more than 2.9 and 3.0 g/cm³ in dry and wet states, respectively. Using additions of zinc stearate in the amount of 0.15% with respect to the weight of the powder, magnets with a density of 7.55 g/cm³, B _r = 14.02 kG, H _c = 7.91 kOe, and (BH)_max = 46.1 MG Oe have been produced.     

粘结剂和添加剂对注射成型各向异性粘结NdFeB磁体的影响(英文)

研究了在取向磁场下由HDDR磁粉注射成型的各向异性粘结NdFeB磁体,分析了粘结剂和添加剂对各向异性粘结NdFeB磁体的密度、磁性能以及抗压强度的影响.通过磁粉表面改性,磁粉的抗氧化性能以及磁体的磁性能都得到提高.比较了6种粘结剂对磁体性能的影响,从中得到比较理想的粘结剂,并且考察了抗氧剂以及润滑剂加入量对于磁体性能的影响.试验中,混炼温度为205～215 ℃,注射温度为265℃,注射压力为5～6 MPa,保压时间为5 s,模具加热温度为80℃.制得的磁体的性能为:Br=0.72 T,iHc=983 kA/m,(BH)max=75 kJ/m3.     

Magnetic properties and thermal stability of anisotropic bonded Nd-Fe-B magnets by warm compaction

Anisotropic bonded magnets were prepared by warm compaction using anisotropic Nd-Fe-B powder. The forming process, magnetic properties, and temperature stability were studied. The results indicate that the optimal temperature of the process, which was decided by the viscosity of the binders, was 110℃. With increasing pressure, the density of the magnets increased. When the pressure was above 700 MPa, the powder particles were destroyed and the magnetic properties decreased. The magnetic properties of the anisotropic bonded magnets were as follows: remanence Br = 0.98 T, intrinsic coercivity iHc=1361 kA/m, and maximum energy product BHmax = 166 kJ/m3. The magnets had excellent thermal stability because of the high coercivity and good squareness of demagnetization curves. The flux density of the magnets was 35% higher than that of isotropic bonded Nd-Fe-B magnets at 120℃ for 1000 h. The flux density of the bonded magnets showed little change with regard to temperature.     

Preparation of high-power permanent magnets from platelike Nd-Fe-B alloys

The microstructure of platelike Nd-Fe-B alloys prepared by rapid quenching from the melt, namely, by the strip casting technique, has been studied. The processes of grain refinement, texture formation, and sintering were optimized. It is shown that the maximum energy product (BH)_max ≥ 50 MGOe can be realized in sintered magnets prepared from the alloy with 29 wt % Nd after a two-step heat treatment. The oxygen content in such magnets does not exceed 0.3 wt %; the degree of texture is α_t = 0.95.     

The magnetic, structure and mechanical properties of rapidly solidified (Nd7Y2.5)-(Fe64.5Nb3)-B23 nanocomposite permanent magnet

The Nd₇Y_2.5Fe_64.5Nb₃B₂₃ nanocomposite permanent magnets in the form of rods with 2 mm in diameter have been developed by annealing the amorphous precursors produced by copper mold casting technique. The phase evolution, structure, magnetic and mechanical properties were investigated with X-ray diffractometry, differential scanning calorimetry, electron microscopy, magnetometry and universal uniaxial compression strength techniques. The heat treatment conditions under which the magnets attained maximum magnetic and mechanical properties have been established. The results indicate that magnet properties are sensitive to grain size and volume content of the magnetic phases present in the microstructure. The composite microstructure was mainly composed of soft α-Fe (20-30 nm) and hard Nd₂Fe₁₄B (45-65 nm) magnetic phase grains. The maximum coercivity of 959.18 kA/m was achieved with the magnets annealed at 760 °C whereas the highest remanence of 0.57 T was obtained with the magnets treated at 710 °C. The optimally annealed magnets possessed promising magnetic properties such as _jH_c of 891.52 kA/m, B_r of 0.57 T, M_r/M_s = 0.68, (BH)_max of 56.8 kJ/m³ as well as the micro-Vickers hardness (H_v) of 1138 ± 20 and compressive stress (σ_f) of 239 ± 10 MPa.     

Preparation of sintered Nd-Fe-B magnets by pressless process

Pressless process used for the preparation of sintered Nd-Fe-B magnets has been studied. The effect of the average particle size D _av, filling density ρ_f, and powder-texturing conditions for obtaining density ρ and desired magnetic hysteretic properties of sintered magnets has been investigated for both traditional technology (TT) and low-oxygen technology (LOT). The ρ_f magnitude ensuring the optimum relation between the density ρ of sintered magnets and their degree of texture was shown to be 2.5–3.0 and 2.2 g/cm³ for the TT and LOT, respectively. At lower ρ_f magnitudes, no required density of sintered magnets is reached, whereas at higher filling densities, a low level of texture and low remanence are realized. Optimum parameters of pulsed field inducing the high degree of texture in powders have been determined. The following properties were achieved for magnets prepared by pressless LOT: B _r ≥ 14.2 kG, H _c ≥ 8 kOe, and (BH)_max ≥ 47.9 MG Oe.     

Structure and magnetic properties of strontium ferrite anisotropic powder with nanocrystalline structure

The phase composition, nanocrystallite size, lattice microstrain and particles morphology of a SrFe₁₂O₁₉ powder subjected to milling and subsequent annealing were studied by various methods. The investigations showed that the high-temperature annealing of the preliminarily milled powder resulted in the increase in the coercive force (μ₀Н_сi) of the SrFe₁₂O₁₉ powder up to 0.4 T owing to the formation of nanocrystalline structure (D ∼ 10³ nm) with low lattice microstrains. However, the annealed powder cannot be textured in an applied magnetic field because of random orientations of the crystallites in powder particles. A processing technique, which includes the low-temperature annealing of powder in an applied magnetic field, was suggested. It allowed us to produce the anisotropic powder of the strontium ferrite with the nanocrystalline structure that ensures the high coercive force of the powder (∼0.4 T) and possibility of the powder texturing in the magnetic field. The prepared samples textured in a magnetic field exhibit the higher both remanence (by a factor of 1.4) and energy product (by a factor of 2.1) as compared to those of isotropic SrFe₁₂O₁₉ samples.     

Hot-deformed Nd-Fe-B magnets fabricated by dynamic loading with a high maximum energy product

To enhance the degree of c-axis alignment of hot-deformed Nd-Fe-B magnets, a dynamic loading process was applied during the hot deformation process with a total thickness reduction of 75%. The effects of processing temperature on magnetic properties and texture alignment were analyzed based on the magnetic properties measurement and microstructure characterization. The extent of c-axis alignment calculated by Half-Gaussian model shows that the orientation deviation decreased to 7.9° when processed at 675 °C. This corresponds to a remanence of 1.49 T and a high maximum energy product (BH)_max of 422 kJ/m³. The activation energy of grain growth during hot deformation is estimated to be 125.8 ± 0.2 kJ/mol. The coercivity-grain size relationship of the samples shows an increase in coercivity with decreased grain size, whose slope is consistent with a previous report.     

Enhancing magnetic properties of anisotropic NdDyFeCoNbCuB powder by applying magnetic field at high temperature during hydrogen desorption

Anisotropic powder was prepared with precursor (NdDy)-(FeCoNbCu)-B sintered magnets by hydrogen decrepitation, desorption, and subsequent annealing treatment. The hydrogen desorption was performed in magnetic fields of 0, 1, 3, and 5 T. The orientation of tetragonal phase grains of the powder was evaluated from the hysteresis loops measured by extraction magnetometer. Residual hydrogen content of the powder was evaluated by thermal-magnetic analysis. The powder with H _cj, B _r, and (BH)_max of 1138 kA·m⁻¹, 1.029 T, and 172.5 kJ·m⁻³, respectively, was achieved under the condition of the magnetic field of 3 T. Magnetic properties of the powder, especially, the remanence of the powder, are enhanced upon magnetic fields, which is due to better orientation of powder particles and less residual hydrogen in the powder resulted from the magnetic field during the hydrogen desorption process.     

Composition dependence of magnetic properties of directly quenched Nd-Fe-Ti-Zr-B bulk magnets

Magnetic properties, phase evolution, and microstructure of directly quenched Nd_yFe_97−y−zTi_3−xZr_xB_z (x = 0-3; y = 7-10; z = 14-19) bulk magnets of 0.9 mm in diameter have been investigated. Proper Zr substitution for Ti and appropriate Nd and B contents modify the magnetic phases constitution and refine the grain size from 200-250 nm to 50-100 nm. Consequently, the magnetic properties of the rods are enhanced remarkably from _iH_c = 6.2 kOe and (BH)_max = 5.6 MGOe for Zr-free rods to _iH_c = 6.7-13.5 kOe and (BH)_max = 6.7-8.2 MGOe for Zr-substituted Nd_yFe_97−y−zTi_3−xZr_xB_z rods (x = 0.5-2; y = 8-10; z = 14-16). The optimum magnetic properties of B_r = 6.6 kG, _iH_c = 9.6 kOe and (BH)_max = 8.2 MGOe were achieved for Nd_9.5Fe_72.5Ti_2.5Zr_0.5B₁₅ alloy.     

Influence of heat treatment on fracture and magnetic properties of radially oriented Sm2Co17 permanent magnets

The quenching, fracture and aging treatment of radially oriented Sm2Co17 ring magnets were investigated. The results indicate that the ring magnets have obvious anisotropy of thermal expansion, which easily leads to the splits of the magnets during quenching. The fracture is brittle cleavage fracture. The difference （Aa） of the expansion coefficient reaches the maximum value at 800-850 ℃. So, various quenching processes at different steps are adopted in order to reduce the splits. When the magnets are aged, 1：5 phase precipitates from the 2：17 matrix phase and forms a cellular microstructure with 2：17 phase. BHmax and JHc reach the maximum value 226 kJ/m^3 and 2 170 kA/m after being aged at 850 ℃ for 4 h and 8 h, respectively. The aging treatment at 850 ℃ has little influence on remanence（Br）, which can always keep a high value （≥1.0 T）. Through appropriate heat treatment, the ring magnets have uniform cellular microstructure and excellent magnetic properties： Br ≥ 1.0T, JHc ≥2 100 kA/m, BHmax ≥ 220 kJ/m^3.     

Properties of the GdTX (T = Mn, Fe, Ni, Pd, X = Al, In) and GdFe6Al6 intermetallics

The magnetic and magnetocaloric properties of GdTX (T = Mn, Fe, Ni, Pd, X = Al, In) and GdFe₆Al₆ ternary compounds for possible applications in magnetic refrigeration have been investigated. Magnetization measurements have been performed in the temperature range of 2-400 K and magnetic field range of 0-7 T. The magnetic entropy changes ΔS_m have been calculated indirectly from the magnetization measurements. The calculated values of entropy change ΔS_m for examined compounds amount −13.63 J/K kg, −13.05 J/K kg, −6.13 J/K kg, −3.72 J/K kg, −1.38 J/K kg and −0.94 J/K kg, respectively, for GdNiAl, GdPdAl, GdPdIn, GdFeAl, GdFe₆Al₆ and GdMnAl at 7 T.     

Large magnetic entropy change near room temperature in La0.7(Ca0.27Ag0.03)MnO3 perovskite

In this paper, the magnetic properties and magnetocaloric effect (MCE) of La_0.7(Ca_1−xAg_x)_0.3MnO₃ (x = 0, 0.1, 0.2, 0.7, and 1) powder samples are reported. Our polycrystalline compounds were synthesized using the solid state reaction method at high temperature. Magnetization measurements versus temperature showed that all our samples exhibited a paramagnetic to ferromagnetic transition with decreasing temperature. The Curie temperature, T_C, has been found to increase from ∼250 K for x = 0-270 K for x = 1. Ag doping weakens the first order phase transition, and at higher Ag doping, the phase transition is of second order. For the La_0.7(Ca_0.27Ag_0.03)MnO₃ composition, the maxima of the magnetic entropy changes from the applied magnetic field (ΔS_M) at 2 and 5 T are about 4.5 and 7.75 J/kg K, respectively, at the Curie temperature of ∼263 K. The relative cooling power (RCP) values without hysteresis loss are about 102 and 271 J/kg for the applied fields of 2 and 5 T, respectively. Due to the large ΔS_M, large RCP, and high Curie temperature, La_0.7(Ca_0.27Ag_0.03)MnO₃ is promising for application in potential magnetic refrigeration near room temperature.     

钕铁硼磁粉HDDR工艺各向异性生成机理研究

本文对钕铁硼速凝薄带进行“氢化-歧化-脱氢-复合”工艺(HDDR)处理,研究了歧化时间、脱氢压力对HDDR磁粉磁性能的影响及磁各向异性的产生机理。通过XRD对其进行物相表征,SEM观察微观形貌及磁性能测试,结果表明：歧化时间决定了HD工艺后磁粉材料中歧化相和残余母相Nd₂Fe₁₄BH_1.04的含量,残余母相能够更好地将母相的织构信息传递下去,使得新相Nd₂Fe₁₄B有很强的c轴织构,磁粉在歧化时间为40 min时各向异性达到最佳,DOA=0.55。而脱氢压力主要作为晶体生长的驱动力,压力在0.01 MPa时驱动力过大,导致脱氢之后晶粒生长方向随机,c轴织构不明显,生成的新相Nd₂Fe₁₄B的各向异性较弱；磁粉在脱氢压力为0.03 Mpa时各向异性得到显著增强,DOA=0.53。     

Anisotropic magnetocaloric effect in TbNiAl

We present study of the anisotropic magnetocaloric effect in TbNiAl crystallizing in the hexagonal ZrNiAl-type structure. TbNiAl orders antiferromagnetically below T_N = 47 K and undergoes second magnetic phase transition to another antiferromagnetic structure at T₁ = 23 K. Magnetization and specific heat measurements on single crystal revealed strongly anisotropic magnetocaloric effect. The large effect occurs for field applied along the hexagonal c-axis whereas the entropy change is almost zero for the perpendicular field direction. Plateau-like character of the determined temperature change is observed between T_N and T₁.     

Phase, structural, and magnetocaloric properties of high temperature annealed LaFe11.6Si1.4BX

The phase relation, microstructural, hysteresis, Curie temperature, and magnetocaloric effects of LaFe_11.6Si_1.4B_x (x = 0.1, 0.2, 0.3, 0.4, and 0.5) prepared by arc-melting and then annealed at 1373 K (1.5 h) + 1523 K (5 h) were investigated. It was found that the main phase is NaZn₁₃-type phase, the impurity phases include α-Fe, Fe₂B, and small amount of La₅Si₃. The boron atom can dissolve into the crystal lattice of LaFe_11.6Si_1.4B_x to form interstitial solid solution, but the content of solid solution is not up to x = 0.5. For LaFe_11.6Si_1.4B_x (x = 0.1, 0.3, and 0.5) compounds, the Curie temperature T_C increases from 190.6 to 198.3 K with the increasing of B content from x = 0.1 to 0.5. The first order magnetic transition behavior becomes weaker and magnetic entropy change ΔS_M (T, H) drops with the increasing of B content, respectively. However, ΔS_M (T, H) still remains a large value, 11.18 J/kg K, when x reaches to 0.5 at 0-2 T. An attractive feature is that both thermal and magnetic hysteresis can be reduced remarkably by introducing B. The maximum magnetic hysteresis loss near T_C drops from 22.52 to 4.95 J/kg when the content of B increases from x = 0.1 to 0.5.     

双主相混合稀土基RE-Fe-B磁体的磁性能和抗腐蚀性改进

为了实现稀土资源的平衡应用且降低RE-Fe-B稀土永磁材料的价格,针对混合稀土基永磁材料进行研究,分别采用单、双主相工艺制备了名义成分[(Pr,Nd)_1-xMM_x]_30.3(Fe,Co)_balM_0.73B_0.98 （x=0.3,0.5和0.7,质量分数）的磁体,对比研究其磁性能和抗腐蚀性。研究发现：双主相工艺制备的磁体相比单主相工艺制备的同成分磁体展现了优越的磁性能和抗腐蚀性。当x=0.5,双主相磁体的磁性能为B_r=1.308 T,H_cj=799.98 kA/m和(BH)_max=325.6436 kJ/m³,远高于同成分的单主相磁体的性能（B_r=1.297 T,H_cj=746.8868 kA/m 和(BH)_max=317.8428 kJ/m³）。这种改进源于富稀土相分布的改进以及主相晶粒间和晶粒内部耦合作用的增强。当双主相磁体暴露在湿热环境下时,磁体中不仅存在富稀土相腐蚀,也存在主相晶粒的腐蚀成粉现象,这主要是由于富稀土相与水蒸气和氧气反应时产生氢气,导致主相晶粒被氢化,由于主相晶粒间和晶粒内部的镧铈分布差异,产生大的应力,导致其表现出区别于单主相磁体的腐蚀行为。     

Grain boundary and interface chemistry of an Nd-Fe-B-based sintered magnet

The compositions of grain boundaries (GBs) and other interfaces surrounding Nd₂Fe₁₄B grains in commercial Nd-Fe-B sintered magnets have been investigated by laser-assisted three-dimensional atom probe to understand the mechanism of the coercivity enhancement by post-sinter annealing. While only a slight segregation of Nd and Pr to the GBs was confirmed in the as-sintered sample, a thin Nd-rich amorphous phase layer was observed along the GBs with Cu segregation to the interfaces in the annealed sample. The segregation of Cu to NdO_x/Nd₂Fe₁₄B interfaces was also found, suggesting that the Nd₂Fe₁₄B grains are enveloped by a Cu-enriched layer after the annealing. The concentration of Fe + Co in the thin GB layer was found to be as high as 65 at.%, and a model amorphous film processed by sputtering with the same composition as the thin GB layer was found to be ferromagnetic. Ferromagnetic behavior of the thin GB layer suggested that Nd₂Fe₁₄B grains are magnetically coupled. The coercivity mechanism of the sintered magnets is discussed based on these new findings.     

Strong correlation between structural, magnetic and transport properties of non-stoichiometric Sr2FexMo2−xO6 (0.8 ≤ x ≤ 1.5) double perovskites

Sr₂Fe_xMo_2−xO₆ (x = 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 and 1.5 wt.%) (SFMO) double perovskite oxides of different compositions have been prepared by sol-gel method. These materials were subjected to X-ray diffraction and found that crystal structure changes from tetragonal to cubic around x = 1.2 wt.%. Lattice parameters and unit cell volume have been calculated using X-ray diffraction data. Magnetization studies have been carried out using Vibrating Sample Magnetometer ranging from −15 kOe to +15 kOe and saturation magnetization (M_s) has been determined. Electrical resistivity and magnetoresistance studies have been carried out in the magnetic field range of −40 kOe to +40 kOe keeping the temperature constant at 5, 150 and 300 K using standard four-probe method. Resistivity studies have also been carried out in the temperature ranging from 5 to 300 K keeping the magnetic field constant at 0, 10, 20 and 40 kOe. Maximum degree of Fe/Mo ordering (η_max) of SFMO has been calculated and compared with magnetic and transport properties. It has been found that there is a strong correlation between 3 parameters η_max, M_s and MR (%), i.e. all of them show a maximum at x = 1.0 wt.% and decreases as x deviates from 1.0 in SFMO. It has been also found that there is a different resistivity behavior between x ≤ 1.2 wt.% and x > 1.2 wt.% samples of SFMO. Semiconductor metal transition temperature was found to be maximum at x = 1.0 wt.%.     

Enthalpy of formation of selected mixed oxides in a CaO-SrO-Bi2O3-Nb2O5 system

The heats of drop-solution in 3Na₂O + 4MoO₃ melt at 973 K and 1073 K for calcium and strontium carbonates, Bi₂O₃, Nb₂O₅ and several stoichiometric mixed oxides in CaO-Nb₂O₅, SrO-Nb₂O₅ and Bi₂O₃-Nb₂O₅ systems were measured using a Setaram Multi HTC-96 calorimeter. The values of enthalpy of formation from constituent binary oxides at 298 K, Δ_oxH, were derived for the mixed oxides under investigation: Δ_oxH(CaNb₂O₆) = −132.0 ± 23.8 kJ mol⁻¹, Δ_oxH(Ca₂Nb₂O₇) = −208.0 ± 31.9 kJ mol⁻¹, Δ_oxH(SrNb₂O₆) = −167.9 ± 19.1 kJ mol⁻¹, Δ_oxH(Sr₂Nb₂O₇) = −289.2 ± 37.5 kJ mol⁻¹ and Δ_oxH(BiNbO₄) = −41.9 ± 11.1 kJ mol⁻¹. Additionally, the values Δ_oxH for other mixed oxides with different stoichiometries were estimated on the basis of these experimental results.