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     

$hbox{Mg}_{1-{rm x}}hbox{Co}_{rm x}hbox{Fe}_{1.98}hbox{O}_{4}$ Ceramics With Promising Magnetodielectric Properties for Antenna Miniaturization

We have studied the effects of concentration of cobalt and sintering temperature on the complex relative permittivity and permeability of MgFe_1.98O₄ ferrite ceramics. All samples were doped with 3 wt% Bi₂O₃ to improve the sintering properties of the Mg_1-xCo_xFe_1.98O₄ ceramics and thus attain a low dielectric loss tangent. X-ray diffraction data indicated that the ferrite samples all have a single-phase spinel structure and that there was no reaction between the ferrite and Bi₂O₃. In terms of microstructure development and grain growth, the effect of Bi₂O₃ is much more pronounced than that of Co. At a given concentration of Co, the magnetic properties can be fairly explained by a magnetic circuit model. The relationship between static permeability and the concentration of Co can be understood by using the single-ion model combined with the local uniaxial anisotropic model. Among the samples we prepared, Mg_0.96Co_0.04Fe_1.98O₄ sintered at 1000degC for 2 h has almost equal real permeability and permittivity-both approximately 10 - as well as sufficiently low dielectric and magnetic loss tangent over a range 3 to 30 MHz [the high-frequency (HF) band]. These properties that should be useful for miniaturization of HF antennas.     

Perpendicular Magnetic Tunnel Junctions with CoFe/Pd Multilayer Electrodes and an MgO Barrier

We studied the magnetic and magnetoresistance characteristics of pseudospin-valve magnetic tunnel junctions (MTJs) based on CoFe/Pd multilayer electrodes with perpendicular magnetic anisotropy and an MgO barrier. The MTJs at annealing temperature (T _a) of 473 K showed a tunnel-magnetoresistance (TMR) ratio of 1.5%. An fcc (111)-oriented texture of the bottom and top Co₉₀Fe₁₀/Pd multilayer electrodes, together with an imperfectly crystallized MgO, were revealed by cross-sectional TEM images. The TMR properties of perpendicular MTJs with a Co₂₀Fe₆₀B₂₀ or Co₅₀Fe₅₀ layer inserted between the CoFe/Pd multilayer electrodes and the MgO barrier were also studied. The TMR ratio with Co₂₀Fe₆₀B₂₀ insertion was 1.7% at T _a= 473 K and monotonically decreased at T _a over 523 K. The TMR ratio with Co₅₀Fe₅₀ insertion increased up to 3% at T _a= 573 K and then decreased to 0.4% at T _a= 598 K. The influence of the Pd layer on CoFeB was studied by using the simplified structures of Pd/CoFeB/MgO/CoFeB/Pd and Ta/CoFeB/MgO/CoFeB/Ta with inplane anisotropy. A former structure with Pd resulted in reduced TMR ratio which decreases with increasing T _a, whereas MTJs with a Ta-based structure showed a monotonic increase of a TMR ratio. The low TMR ratio observed in Pd-containing structures appears to result from crystallization of CoFeB in an unfavorable crystal orientation.     

Stability of the structure corresponding to the prepeak and amorphous Al90Tm5Ce5 alloys

The stability of amorphous Al₉₀Fe₅Ce₅ and Al₉₀Ni₅Ce₅ alloys and the stability of the structure corresponding to the prepeak during annealing process were investigated. Also the ageing effects of these alloys were investigated. Both the amorphous Al₉₀Fe₅Ce₅ and Al₉₀Ni₅Ce₅ alloys crystallize by two stages. The crystallization onset temperature for amorphous Al₉₀Fe₅Ce₅ alloys is much higher than that of the amorphous Al₉₀Ni₅Ce₅ alloys. The structure corresponding to the prepeak for amorphous Al₉₀Fe₅Ce₅ alloys is stable. However, it is not stable for amorphous Al₉₀Ni₅Ce₅ alloys, even decomposes at room temperature. By ageing effects, fcc Al is easily precipitated from amorphous matrix for the amorphous Al₉₀Ni₅Ce₅ alloys, whereas the amorphous Al₉₀Fe₅Ce₅ alloys is stable at room temperature. The stability of the structure corresponding to the prepeak strongly relates to the stability of the amorphous alloys.     

Plastic deformation of Al13Fe4 particles in Al–Al13Fe4 by high-speed compression

Spray-formed Al–Fe alloys having undergone high-speed deformation were examined under a high-voltage electron microscope. Two types of specimens were examined; one containing fine Al₁₃Fe₄ particles, and the other containing large particles. In the former specimen, deformation is found to proceed in three patterns, depending on specimen thickness and strain rate: (1) without deformation of the Al₁₃Fe₄; (2) breaking of the Al₁₃Fe₄; or (3) melting of the Al₁₃Fe₄. Local melting is found to alter some of the Al₁₃Fe₄ particles, to impart five-fold symmetry in diffraction or an amorphous structure. In the latter specimen, introduction of glide dislocations enabled us to determine a shear system in the mc102 monoclinic c2/m crystal of Al₁₃Fe₄. On the bases of these observations, the mechanism of high-speed deformation is discussed while taking into account the highly stressed and/or heated states of Al₁₃Fe₄ embedded in Al matrix.     

改进HDDR工艺制备NdFeCoZrBGa各向异性磁粉

HDDR(氢化-歧化-脱氢-重组)工艺是一种用于生产各向异性Nd2Fe14B基磁粉的特殊方法。本文主要研究了添加微量含金元素Ga、采用改进HDDR工艺(即在HD处理及高真空脱氢处理之间加上低真空脱氢处理)对Nd11.2Fe66.5-xCo15.4B6.8Zr0.1Gax(x=0、0．1、0．3、0．5、1．0)合金磁性能的影响规律。结果表明．改进HDDR工艺对于提高磁粉性能,细化主相晶粒尺寸非常有效。微量合金元素Ga的添加可显著地改变材料歧化分解的特征,同时可提高磁粉的磁性能。由改进HDDR工艺制得磁粉主相晶粒尺寸明显小于由传统HDDR工艺制得磁粉主相晶粒尺寸。     

P型Si80Ge20B0.6-SiC纳米复合材料的微观结构与热电性能研究

采用感应熔炼、球磨与放电等离子烧结的方法制备了SiC第二相均匀分布的Si₈₀Ge₂₀B_0.6-SiC纳米复合热电材料。系统研究了细化Si₈₀Ge₂₀B_0.6晶粒尺寸与复合SiC纳米颗粒对材料热电性能的影响。球磨导致的Si₈₀Ge₂₀B_0.6晶粒尺寸的降低显著增加了材料的晶界数量, 进而增强了晶界对中长波声子的散射, 能够有效降低材料的晶格热导。Si₈₀Ge₂₀B_0.6基体中均匀分布的纳米SiC颗粒提供了额外的散射中心和界面,可进一步增强声子散射,降低材料的晶格热导。在纳米结构化与SiC纳米复合的共同作用下, 材料在1000 K 时热电优值ZT达到了0.62, 较基体提高了17%。证明纳米结构化与纳米复合方法能够共同作用于硅锗合金, 提高其热电性能。     

The microstructure and magnetic properties of NdFeB magnets directly solidified at a low cooling rate

Nd_12.5Fe₈₂B_5.5 ribbons have been prepared by a melt spinning technique at a wheel speed ranging from 5 to 22 m/s. It was found that the wheel speed v_R dramatically influences the microstructure and magnetic properties of the ribbons. At an optimized v_R, a structure with single-phase Nd₂Fe₁₄B and an enhanced coupling between grains give rise to excellent magnetic properties. For example, the coercivity, remanence ratio, and maximum energy product of the best sample quenched at a wheel speed of 13 m/s are 1227.4 kA/m, 0.76, and 182.6 kJ/m³, respectively. In comparison with the samples from under- and over-quenched conditions and all the samples with annealing, the as-quenched sample fabricated at the optimized wheel speed has the best magnetic properties.     

退火温度对无镁La-Y-Ni系A2B7型合金相结构和电化学性能的影响

用XRD、SEM、EDS和电化学测试方法研究了退火温度对A₂B₇型La_0.33Y_0.67Ni_3.25Mn_0.15Al_0.1储氢合金微观组织和电化学性能的影响规律。结果表明, 合金铸态组织由2H-Ce₂Ni₇、3R-Gd₂Co₇、CaCu₅和3R-Ce₅Co₁₉型相组成; 随退火温度(850~950℃)升高, Ce₂Ni₇型主相丰度和晶胞体积逐渐增加, 至950℃退火后, CaCu₅和Gd₂Co₇型相基本消失, 主相Ce₂Ni₇型相丰度和晶胞体积均达到最大值; 退火温度≥950℃时, Ce₂Ni₇型和Ce₅Co₁₉型相丰度分别又有所减少和增加。950℃退火合金具有较低的放氢平台压(1.92~8.70 kPa)和较高的电化学放电容量(371 mAh/g), 经100次充放电循环后其容量保持率S₁₀₀达到89%。退火合金电极的HRD性能均得到不同程度的提高, 其中950℃退火合金具有最佳的大电流放电性能(HRD₉₀₀=83.4%)。氢在合金中的扩散是影响其高倍率放电性能的控制因素。     

稀土氧化物Pr2O3掺杂对高压ZnO压敏电阻性能的影响

采用低温固相化学反应法制备了Pr₂O₃掺杂的ZnO纳米复合粉体, 并用此粉体在不同烧结温度下制备了高压ZnO压敏电阻。采用X射线衍射、 比表面测试、 透射电镜、 扫描电镜等手段对制备的ZnO纳米复合粉体及高压ZnO压敏电阻进行了表征, 并与未掺杂ZnO压敏电阻进行了对比研究, 探讨了稀土氧化物Pr₂O₃掺杂对高压ZnO压敏电阻电性能的影响机制。结果表明: 较低的烧结温度(1030～1130 ℃)时, 掺杂的稀土氧化物Pr₂O₃偏析于ZnO晶界中, 有活化晶界、 促使晶粒生长的作用; 同时, Pr₂O₃掺杂导致1080 ℃烧结的ZnO压敏陶瓷体中晶体相互交织形成晶界织构, 比未掺杂的更均匀和致密, 这有助于高压ZnO压敏电阻晶界性能的改善, 从而提高其综合电性能。当烧结温度为1080 ℃时, Pr₂O₃掺杂的高压ZnO压敏电阻的综合电性能最佳: 电位梯度为864.39 V/mm, 非线性系数为28.75, 漏电流为35 μA。     

Magnetic anisotropies in single and multilayered thin films grownby bowed-substrate sputtering

Thin-film structures composed of nearly nonmagnetostrictive single-layer Co₇₆Fe₄B₂₀ or magnetostrictive Fe₈₀B₂₀ and Co₇₅Si₁₅B₁₀ amorphous layers have been deposited on bowed glass substrates using the RF-sputtering technique. The fabrication procedure induces a postdeposition compressive stress in the thin-film structure when the sample is retrieved from an arching device in the sputtering chamber. This results in an induced magneto-elastic anisotropy that governs the magnetic easy axis of the film, depending on the sign of the magnetostriction constant of each layer. Particular attention is paid here to heterogeneous structures made of bi- or multilayers with magnetic easy axis oriented in a different direction in each layer. Bulk magnetic properties were evaluated from hysteresis loops and thermomagnetization measured by vibrating sample magnetometry (VSM) and quantum interference device (SQUID) magnetometry. Magnetic domain walls and out-of-plane magnetized domains were observed by a Kerr imaging system and magnetic force microscopy. The combination of microstructure and strains induced in the layers determines the orientation of the observed magnetic anisotropies, which vary from high in-plane anisotropies up to out-of-plane orientations for selected films. The results, which provide reassurance that effective anisotropies are induced in each of the layers, are discussed in terms of the interactions between magnetic phases with different induced easy magnetization axes     

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.     

Comparison of hydrogen storage characteristics between as-cast and melt-spun TiCr1.1V0.5Fe0.1Mn0.1 alloys

Hydrogen storage characteristics of as-cast and melt-spun TiCr_1.1V_0.5Fe_0.1Mn_0.1 alloys were investigated by pressure–composition–temperature (PCT) tests, X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD showed that both the as-cast and the melt-spun alloys were similarly consisted of V based BCC phase and Ti_1.07Cr_1.93 phase. However, PCT tests showed that the melt-spun alloy, with larger hysteresis between hydrogen absorption and desorption, had higher hydrogen storage capacity than the as-cast alloy. More interestingly, the phase compositions of the two fully hydrogenated alloys were entirely different. The as-cast and the melt-spun alloys should have different atomic motion mechanisms during the course of hydrogenation.     

Comparative study of martensitic transformation behavior of NiAlMn and NiAlMnFe high temperature shape memory alloys

A comparative study of microstructure and martensitic transformation (MT) behavior of Ni₅₉Al₁₁Mn₃₀ and Ni₆₀Al₁₉Mn₁₆Fe₅ high temperature shape memory alloys (SMAs) has been performed by means of differential scanning calorimetry (DSC), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDXS), optical microscopy, and micro-hardness testing. The MT temperature (MTT) of Ni₅₉Al₁₁Mn₃₀ alloy is higher than that of Ni₆₀Al₁₉Mn₁₆Fe₅ alloy, and both alloys’ MTT increases with increasing annealing temperature. The temperature hysteresis and hardness of Ni₅₉Al₁₁Mn₃₀ alloy are smaller than that of Ni₆₀Al₁₉Mn₁₆Fe₅ alloy. The MT behavior of Ni₆₀Al₁₉Mn₁₆Fe₅ is sensitive to aging temperature and its MTT and hysteresis decrease with increasing aging temperature. However, the MT behavior of Ni₅₉Al₁₁Mn₃₀ alloy is not sensitive to aging temperature. The MT stabilization effects appear in both alloys during thermal cycles. This stabilization effect vanishes from the second thermal cycle. The quenched microstructure of Ni₅₉Al₁₁Mn₃₀ and Ni₆₀Al₁₉Mn₁₆Fe₅ alloys is M plus gamma phase, in which the volume fraction of gamma phase is about 40 and 20%, respectively, and the microhardness of M is higher than that of gamma phase. No aging effects were found in both alloys after aging at 400 °C.     

Chemical vapour deposition of praseodymium oxide films on silicon: influence of temperature and oxygen pressure

Metal-organic chemical vapour deposition (MOCVD) of various phases in PrO_x system has been studied in relation with deposition temperature (450–750 °C) and oxygen partial pressure (0.027–100 Pa or 0.2–750 mTorr). Depositions were carried out by pulsed liquid injection MOCVD using Pr(thd)₃ (thd = 2,2,6,6-tetramethyl-3,5-heptanedionate) precursor dissolved in toluene or monoglyme. By varying deposition temperature and oxygen partial pressure amorphous films or various crystalline PrO_x phases (Pr₂O₃, Pr₇O₁₂, Pr₆O₁₁) and their mixtures can be grown. The pure crystalline Pr₂O₃ phase grows only in a narrow range of partial oxygen pressure and temperature, while high oxygen pressure (40–100 Pa) always leads to the most stable Pr₆O₁₁ phase. The influence of annealing under vacuum at 750 °C on film phase composition was also studied. Near 90% step coverage conformity was achieved for PrO_x films on structured silicon substrates with aspect ratio 1:10. In air degradation of Pr₂O₃ films with transformation to Pr(OH)₃ was observed in contrast to Pr₆O₁₁ films.     

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.     

CoFe2O4-Co3Fe7纳米粒子及CoFe2O4/多孔碳的制备及其电磁性能研究

在5% H₂+95% N₂气氛下,还原CoFe₂O₄纳米粒子制备了CoFe₂O₄-Co₃Fe₇纳米粒子;以焙烧黄麻纤维得到的多孔碳纤维为碳源用水热法将CoFe₂O₄纳米粒子负载到多孔碳中,制备出CoFe₂O₄/多孔碳。使用X射线衍射仪、扫描电子显微镜、透射电子显微镜、拉曼光谱仪、同步热分析仪等手段对材料进行表征,并使用矢量网络分析仪测量了复合材料的电磁参数和微波吸收性能。结果表明,CoFe₂O₄-Co₃Fe₇纳米粒子和CoFe₂O₄/多孔碳的微波吸收性能明显优于CoFe₂O₄纳米粒子。CoFe₂O₄-Co₃Fe₇纳米粒子的有效频宽(反射损耗<-10 dB的频率宽度)可达4.8 GHz。CoFe₂O₄/多孔碳的有效频宽可达6 GHz,覆盖了整个Ku波段(12~18 GHz)。这些材料优异的微波吸收性能,可归因于合适的介电常数、大的介电损耗、多孔结构以及介电损耗和磁损耗的协同作用。     

放电等离子烧结技术制备Fe78Si13B9块体非晶纳米晶磁性材料

通过高能球磨技术制备了Fe₇₈Si₁₃B₉磁性非晶合金粉体,采用XRD和DSC分析了Fe₇₈Si₁₃B₉非晶合金粉体的相组成、玻璃转变温度T_g、开始晶化温度 T_x 和晶化峰温度T_p;利用放电等离子烧结（SPS）技术在不同烧结温度下制备了块体磁性非晶纳米晶合金试样,利用XRD、SEM、Gleeble3500、VSM等分析了不同烧结温度下烧结块体试样的相转变特性、微观形貌、力学性能和磁学性能。结果表明,在500 MPa的烧结压力下,随着烧结温度的升高,烧结试样中的非晶相开始逐渐晶化,烧结试样的致密度、抗压强度、微观硬度、饱和磁化强度均显著提高;在500 MPa的烧结压力和823.15 K的烧结温度下,获得了密度为6.6 g/cm³,抗压强度为1500 MPa,饱和磁化强度为1.3864 T的非晶纳米晶磁性材料。