Short range order of the amorphous Fe−B powders prepared by borohydride reduction

Ultrafine Fe?B amorphous alloy powders were prepared by reducing Fe²⁺ ions using KBH₄ and NaBH₄ in aqueous solution. Adjusting technological factors, the amorphous powders around the composition of Fe₆₅B₃₅ can be easily obtained, but in the vicinity of eutectic point (Fe₈₀B₂₀) a certain amount of α-Fe often appears in the samples. From the Mössbauer spectrum, the crystallization products of the Fe₆₃B₃₇ amorphous powder are α-Fe and Fe₂B phases. The measurement of¹¹B spin echo nuclear magnetic resonance (NMR) at 8K showed that Fe₂B-like and Fe₃B-like short range orders (SRO) exist in the amorphous powder of Fe₇₆B₂₄.     

Crystallization of Fe-B amorphous alloy powders produced by chemical reduction

The crystallization behaviour of the Fe?B amorphous alloy powders prepared by the chemical reduction method has been investigated by Mössbauer spectroscopy. In comparison to amorphous ribbons prepared by melt-spinning, a different crystallization behaviour has been observed. After annealing the amorphous samples entirely crystallized into three crystalline phases: α-Fe, Fe₃B, and Fe₂B. In the case of Fe₈₀B₂₀ amorphous alloy ribbons produced by melt-spinning technique eutectic crystallization is commonly observed and results in the crystalline phases: α-Fe and Fe₃B. This kind of crystallization was not observed in the chemically prepared samples. The metastable tetragonal Fe₃B phase transformed completely into α-Fe and Fe₂B after annealing at 973 K for one hour.     

Fe-doped TiO2 prepared by mechanical alloying

The effect of different milling conditions on the formation of Fe-doped TiO₂ powders by mechanical alloying was investigated by Mössbauer spectrometry. The milling conditions investigated were ball to powder weight ratio, milling time, rotation velocity of supporting disc, and the type of starting reactive iron and its concentration. X-ray diffraction shows that high energy mechanical milling of undoped anatase TiO₂ induce the anatase to rutile phase transformation via high pressure srilankite. Mössbauer spectra for the majority of the doped samples were decomposed into one sextet and one or two doublets. The sextets was attributed to the presence of α-Fe or hematite impurities. The doublets were assigned to Fe^3?+? incorporated in the TiO₂ structure, and to the Fe^2?+? located either at the surface or the interstitial sites of TiO₂. A greater incorporation of Fe in the TiO₂ structure was observed when samples were prepared from hematite instead of α-Fe.     

Research on preparing compact bulk nanocomposite Nd2Fe14B/α-Fe magnetic materials by hot extrusion

In this paper, compact bulk nanocomposite Nd₂Fe₁₄B/α-Fe magnetic materials were prepared by hot extrusion of amorphous and nanocrystalline powders, which were prepared by high-energy ball-milling (HEBM) of the Nd₂Fe₁₄ B-type hard magnetic phase with 20 vol% of α-Fe as soft magnetic phase. The extrusion temperature has important influence on magnetic properties and microstructure of magnetic materials. The results show that the grain size of Nd₂Fe₁₄B and α-Fe phase increases steadily with increasing extrusion temperature. Furthermore, optimal extrusion temperature of 1223 K occurs, at which the highest magnetic properties and relative density can be obtained.     

Atom probe study on the bulk nanocomposite SmCo/Fe permanent magnet produced by ball-milling and warm compaction

The microstructure and compositions of the bulk nanocomposite SmCo/Fe permanent magnet were studied using transmission electron microscopy and 3-dimensional atom probe techniques. The excellent magnetic properties were related to the uniform nanocomposite structure with nanometer α-Fe particles uniformly distributed in the SmCo phase matrix. The α-Fe phase contained ∼26 at% Co, and the SmCo phase contained ∼19 at% Fe, confirming that the interdiffusion of Fe and Co atoms between the two phases occurred. The formation of the α-Fe(Co) phase explained why the saturation magnetization of the nanocomposite permanent magnet was higher than that expected from the original pure α-Fe and SmCo₅ powders, which enhanced further the maximum energy product of the nanocomposite permanent magnet.     

<Superscript>57</Superscript>Fe NMR study of amorphous and rapidly quenched crystalline Fe-B alloys

Amorphous and crystalline Fe-B alloys (5–25 at % B) were studied using pulsed ⁵⁷Fe nuclear magneticr esonance at 4.2 K. The alloy samples were prepared from a mixture of the ⁵⁷Fe and ¹⁰B isotopes by rapid quenching from the melt. In the microcrystalline Fe-(5–12 at %) B alloys, the resonance frequencies were measured for local states of ⁵⁷Fe nuclei in the tetragonal and orthorhombic Fe₃B phases and also in α-Fe. The resonance frequencies characteristic of ⁵⁷Fe nuclei in α-Fe crystallites with substitutional impurity boron atoms in the nearest neighborhood were also revealed. In the resonance frequency distribution P(f) in the amorphous Fe-(18–25) at % B alloys, there are frequencies corresponding to local Fe atom states with short-range order of the tetragonal and orthorhombic Fe₃B phases. As the boron content decreases below 18 at %, the P(f) distributions are shifted to higher frequencies corresponding to ⁵⁷Fe NMR for atoms exhibiting a short-range order of the α-Fe type. The local magnetic structure of the amorphous Fe-B alloys is also considered.     

Phase composition at surface of Fe-3%Si alloy

The structure, phase and chemical compositions of surface layers in different depths of Fe-3%Si alloy were investigated. According to the X-ray Photoelectron Spectroscopy (XPS) spectrum (penetration depth of up to ∼ 1nm) of the as-prepared sample, a layer of SiO₂ was present on the top. After the subsequent Ar⁺ sputtering (removing the SiO₂ layer), a segregation of Si atoms and two other phases were observed. The phases were described as the cubic c-FeSi and Fe₃Si. The emission⁵⁷Fe M?ssbauer spectra confirmed a presence of these phases. The α-Fe and solid solution of α-Fe + 1wt.%Si were recognized in the Conversion Electron M?ssbauer spectra (penetration depth ∼ 300nm) while the M?ssbauer spectra taken in scattering geometry with detection of 14.4 keV gamma radiation (scanning depth of ∼ 30 μm) indicate Fe-3wt.%Si solid solution as a main phase. Presented at International Colloquium “M?ssbauer Spectroscopy in Materials Science”, Všemina, Czech Republic, June 1–4, 2004. This work was supported by the Grant Agency of the Academy of Sciences of the Czech Republic (Contract No. IAA1041404).     

Fe-C—Sb合金中液态急冷获得的ε相的分解

本工作用示差热分析法,淬火样品X射线衍射法和Guinier-Lenn透射式高温单色聚焦粉末照相法研究了Fe-C-Sb合金中液态急冷获得的ε相的高温分解过程,实验结果指出,ε相在125℃开始分解,首先分解成ε-Fe₂C,而后在450℃分解成α-Fe,并析出Sb和Fe₃Sb₂,还保留有ε-Fe₂C;在550℃以后ε-Fe₂C转变成Fe₃C,并在770℃时发生Fe的α→γ转变,在800℃时主要组成相为:γFe,Sb,Fe₃C(Fe₃Sb分解);在冷却过程中750℃发生Fe的γ→α转变,冷至室温时的主要组成相是:αFe,Fe₃C,Sb,Fe₃Sb₂。 关键词：     

Short-range order in amorphous ferromagnetic Fe-B alloys

Amorphous and quenched crystalline Fe-B alloys in the composition range of 4–25 at % B were prepared by melt spinning and investigated by ⁵⁷Fe Mössbauer spectroscopy at T = 87 K. The states of iron atoms in the α-Fe phases, including iron atoms having boron atoms in the nearest coordination sphere, and in the orthorhombic (o) and tetragonal (T) Fe₂B phases are detected in the microcrystalline alloys. The short-range order and the local atomic structure of the amorphous Fe-B alloys are determined. The amorphous alloys consist of microregions (clusters) with short-range order of the t- and o-Fe₂B and α-Fe types. The dependence of the content of various types of clusters on the alloy composition is quantitatively estimated.     

Crystallization study of amorphous system Fe84−x W x B16 (x=3; 5)

A complex study of the crystallization process of the amorphous system was carried out by Mössbauer spectroscopy, X-ray diffraction and DTA. Alloy samples crystallized at 600 °C contain the following phases: α-Fe, Fe₃B and solid solution (Fe, W)₃B.     

Phase analysis in α-Fe after high-dose Si ion implantation by depth-selective conversion-electron Mössbauer spectroscopy (DCEMS)

Si⁺ ions of 50 keV in energy were implanted into α-Fe (95% ⁵⁷Fe) with a nominal dose of 5 × 10¹⁷ cm^?2 at 350°C. The depth distribution of the Fe-Si phases formed by ion implantation after annealing at 300 and 400°C for 1 h was studied quantitatively by depth-selective conversion-electron Mössbauer spectroscopy (DCEMS). Ordered Fe₃Si and ε-FeSi was observed.     

NMR study of rapidly quenched crystalline and amorphous Fe-B alloys

Amorphous and microcrystalline Fe-B alloys (4–25 at % B) obtained by rapid quenching of the melt were studied using the pulsed nuclear magnetic resonance (NMR) of ¹¹B nuclei at 4.2 K. Alloy samples were prepared from both a natural isotope mixture and a mixture of the ⁵⁶Fe and ¹¹B isotopes. The NMR spectra were measured as a function of the boron content. The maximum hyperfine fields at the ¹¹B nuclei sites are 25–29 kOe and overlap the values of the hyperfine fields at the ¹¹B nuclei sites in the tetragonal and orthorhombic Fe₃B phases and also in the α-Fe phase containing boron as a substitutional impurity. The short-range order and local atomic structure of the amorphous Fe-B alloys were determined. The amorphous alloys are found to consist of microregions (clusters) with a short-range order similar to that in the tetragonal or orthorhombic Fe₃B phase or the α-Fe phase.     

Characterization of iron nitrides prepared by spark erosion,plasma nitriding,and plasma immersion ion implantation

The effect of the nitrogen uptake in α-iron upon spark erosion in gaseous and liquid ammonia, plasma nitriding, and plasma immersion ion implantation is studied. The resulting phases and hyperfine parameters, measured by the Mössbauer spectroscopy, are discussed from the point of view of initial conditions of their preparation and subsequent heat and/or mechanical treatment. Spark erosion in the ammonia gas produces fine particles with the dominating ferromagnetic α-Fe phase (50%). The 20% of specimen volume form α′-Fe and α′′-Fe₁₆N₂ phases. The last 30% occupy the γ′-Fe₄N, ferro- and paramagnetic ε phases, and γ-Fe(N). Nitriding in the liquid ammonia allows to incorporate the higher content of nitrogen into α-iron particles which results in the formation of paramagnetic ε(ζ)-Fe₂N phase. This phase also dominates the surface of α-iron specimen implanted by nitrogen using plasma immersion ion implantation at 300°C/3 h, where high uptake of nitrogen (approx. 30 at%) is reached. Plasma nitriding at 510°C results in the formation of γ′-Fe₄N phase.     

Influence of Cr content on structure and magnetic properties of Fe-Si-Al-Cr powders

As a kind of soft magnetic metallic material, flaky FeSiAl powders have been studied and used widely. Transition metal chromium can improve the magnetic properties of FeSiAl. This article prepared Fe₈₅Si_9.5-xAl_5.5Cr_x (x=0, 2, 4, 6 wt%) alloys powders by adding chromium to replace silicon in alloys. The morphology and microstructure of alloys powders were studied, electromagnetic parameters were measured and microwave absorption properties in the frequency range from 0.5 to 18 GHz were analyzed. With the increase of Cr content, α-Fe (Al, Si) superlattice phases appeared in alloys powders, and then disappeared. Excessive Cr precipitated from the alloys when its content reaches 6 wt%. The minimum reflection loss (-20 dB) among the four powders was 2 wt% Cr content at the frequency of 11.5 GHz. The peaks of reflection loss shifted to the low frequency range with increase in Cr content.     

Microstructural behavior on particle surfaces and interfaces in Sm2Fe17N3 powder compacts during low-temperature sintering

Sm₂Fe₁₇N₃ sintered compacts were prepared below 450 °C by a high-pressure current sintering technique. The coercivity of the sintered compacts decreased linearly as the sintering temperature increased. Transmission electron microscopic analyses indicated that thin Fe-rich layers containing α-Fe phases were formed just inside the initial oxide layer on the particle surfaces and interfaces in the sintered samples. The generation of α-Fe phases was supposed to cause the coercivity decrease. In addition, X-ray photoelectron spectroscopy analysis revealed that Fe₂O₃ and FeO contained in the oxide layer of the raw powder disappeared subsequent to heat treatment. These results suggested that the α-Fe phases were generated by the oxidation–reduction reaction between the initial iron oxides and the primary Sm₂Fe₁₇N₃ phase but not by thermal decomposition or exogenous oxidation during sintering. This mechanism was supported by the fact that extending the sintering time did not result in any further decrease in the coercivity.     

Local structure of Fe70Cr15B15 X-ray amorphous alloy

The local atomic and magnetic structure of Fe₇₀Cr₁₅B₁₅ X-ray amorphous alloy is studied by means of ¹¹B nuclear magnetic resonance (NMR) and ⁵⁷Fe Mössbauer spectroscopy. It is determined that Fe₈₅B₁₅ and Fe₇₀Cr₁₅B₁₅ X-ray amorphous alloys consist of microregions (nanocrystals) with short-range orders of t-Fe₃B and α-Fe phases. It was found out that chromium atoms in the Fe₇₀Cr₁₅B₁₅ X-ray amorphous alloy are evenly distributed in these two nanocrystals, forming t-(Fe,Cr)₃B and α-Fe(Cr) phases.     

Phase transition in metallic glasses Fe66Co12Si9B13 and Fe66Ni12Si9b13

Phase transitions were analysed during annealing of amorphous metallic glasses Fe₆₆Co₁₂Si₉B₁₃ and Fe₆₆Ni₁₂Si₉B₁₃. They were measured by means of X-ray diffraction, electrical and Hall resistivity methods. Forming crystalline phases were identified. Those for metallic glasses with cobalt are α-Fe, Fe₃B and Co₂B while those with nickel are α-Fe, Fe₂B, Ni₂B.     

Preparation,microstructure, and magnetic properties of a nanocrystalline Nd12Fe82B6 alloy by HDDR combined with mechanical milling

Nanocrystalline Nd₁₂Fe₈₂B₆ (atomic ratio) alloy powders with Nd₂Fe₁₄B/α-Fe two-phase structure were prepared by HDDR combined with mechanical milling. The as-cast Nd₁₂Fe₈₂B₆ alloy was disproportionated via ball milling in hydrogen, and desorption–recombination was then performed. The phase and structural change due to both the milling in hydrogen and the subsequent desorption–recombination treatment was characterized by X-ray diffraction (XRD). The desorption–recombination behavior of the as-disproportionated alloy was investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The morphology and microstructure of the final alloy powders subject to desorption–recombination treatment were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results showed that, by milling in hydrogen for 20 h, the matrix Nd₂Fe₁₄B phase of the alloy was fully disproportionated into a nano-structured mixture of Nd₂H₅, Fe₂B, and α-Fe phases with average size of about 8 nm, and that a subsequent desorption–recombination treatment at 760 °C for 30 min led to the formation of Nd₂Fe₁₄B/α-Fe two-phase nanocomposite powders with average crystallite size of 30 nm. The remanence B_r, coercivity H_c, and maximum energy product (BH)_max of such nanocrystalline Nd₁₂Fe₈₂B₆ alloy powders achieved 0.73 T, 610 kA/m, and 110.8 kJ/m³, respectively.     

Nd-Fe(Co,Nb)-B交换耦合磁体的磁性

用熔体快淬法结合热处理制备了高性能纳米复合永磁合金Nd₉Fe_85.5-xCo_xNb₁B_4.5(0≤x≤16).最佳磁性能对应的成分为Nd₉Fe_81.5Nb₁B_4.5,其永磁性能如下：最大磁能积(BH)_max＝156kJ/m³,剩磁J_r＝1.11T 关键词：     

非晶Fe73.5Cu1Nb3Si13.5B9合金激光纳米化的超精细结构研究

在CO₂激光功率为50—300W、扫描速度为20mm/s、激光散光斑为20mm照射条件下 ，诱导非 晶Fe_735Cu₁Nb₃Si_135B9带中发生结构重组，产生定量纳米α-F e(Si)晶相形成双相组织结构材料. 利用穆斯堡尔谱研究了非晶Fe_735C u₁Nb₃Si_135B₉合金激光纳米化的 超精细结构. 实验结果表明，激光诱导非晶 Fe_735Cu₁Nb₃Si_135B ₉纳米化后，其超精细磁场的分布随 着激光功率变 化由单峰向双峰变化，在高功率辐照时， 出现了双峰分布，并且峰位向高场移动. 高激光 功率辐照非晶Fe_735Cu₁Nb₃Si_{135B9合金纳米晶化相有四种超精细结 构，即2个超精细磁场较小的初晶相和2个超精细磁场较大的纳米晶化相. 其中超精细磁场较 大(17—25MA/m)的α-Fe(Si)相为DO3结构. 关键词： 激光 纳米晶α-Fe（Si) 735}Cu₁Nb< sub>3Si_135B₉')" href="#">非晶Fe_735Cu₁Nb< sub>3Si_135B₉ 超精细结构 超精细磁场