Recoilless fraction, structural, magnetic and thermal properties of Fe73.5Cu1Nb3Si13.5B9 alloy

Differential scanning calorimetry, X-ray diffraction and room temperature Mössbauer spectrum measurements of Fe_73.5Cu₁Nb₃Si_13.5B₉ (Finemet) alloy have been carried out in order to study its structural and magnetic properties as a function of annealing temperature. The DSC profile of as-quenched Finemet showed two exothermic peaks at 530 and 702 °C, corresponding to two crystallization processes. The Finemet alloy remains amorphous at 450 °C with one broad peak in XRD pattern and one broad sextet in Mössbauer spectrum. When the Finemet alloy was annealed at 550 °C, only well indexed body-center-cubic phase was detected. After being annealed at 650 and 750 °C, the XRD patterns showed the coexistence of α-Fe(Si) and Fe-B intermetallic phases with the increase in XRD peak intensities, indicating the growth of crystallites and the decomposition of Fe_73.5Cu₁Nb₃Si_13.5B₉ alloy at elevated temperatures. The Mössbauer spectra of annealed Finemet alloy could be fitted with 4 or 5 sextets and one doublet at higher annealing temperatures, revealing the appearance of different crystalline phases corresponding to the different Fe sites above the crystallization temperature. The appearance of the nanocrystalline phases at different annealing temperatures was further confirmed by the recoilless fraction measurements.     

Effect of thermomagnetic and thermomechanical treatments on the magnetic properties and structure of the nanocrystalline soft magnetic alloy Fe81Si6Nb3B9Cu1

The structural and magnetic states of ribbon samples of the soft magnetic alloy Fe-Si-Nb-B-Cu (6 at % Si) have been investigated after the nanocrystallization at a temperature of 550°C in a constant magnetic field (thermomagnetic treatment), in a field of mechanical tensile stresses (thermomechanical treatment), and without external effects. It has been shown that exposure to a constant magnetic field or a field of mechanical tensile stresses gives rise to a longitudinal anisotropy of magnetic properties. The mag- netic hysteresis loop transforms and becomes close to rectangular. This is accompanied by a significant increase in the residual magnetic induction, which approaches the saturation magnetic induction. While the time required to complete the processes of nanocrystallization is as short as 20 min and, under thermome- chanical treatment, the magnetic anisotropy is induced for 20 min, the time it takes to decrease significantly the coercive force of the alloys under thermomagnetic treatment is substantially longer (up to 60 min). After the thermomagnetic treatment, no lattice strains of α-FeSi nanocrystals have been found. Either they do not exist at all, or their values are within the error of the X-ray diffraction experiment. In the samples subjected to annealing under tensile loading, anisotropic lattice strains of nanocrystals with the values increasing pro- portionally to the applied stress have been revealed. The highest strains reaching 1% have been observed after the annealing under a stress of 860 MPa.     

Finemet合金析出相α-Fe(Si)结构与磁性的第一性原理计算

采用基于密度泛函理论的第一性原理计算方法研究Finemet合金中析出相α-Fe(Si)的晶体结构与磁性,探讨影响立方结构α-Fe(Si)相磁性能的各个因素. 从电子自旋角度出发,分别计算分析了不同比例的Si置换α-Fe超晶格中不同位置的Fe原子后α-Fe(Si)体系的磁性能. 计算结果表明,自旋态密度是影响磁性能的关键因素. 发现Si置换α-Fe超晶格顶角处Fe原子得到的体系比取代体心位置Fe原子的体系磁性要好. 由此可以得出结论,在一定的含量范围内,随着Si含量的增加,Si出现在α-Fe超晶格中顶角位置的概率增大,α-Fe(Si)相的软磁性能提高,与实验结果相符. 本文的研究工作有助于理解Finemet合金的磁性机理. 关键词： Finemet合金 磁性能 第一性原理 态密度     

X-ray diffraction studies of the structure of nanocrystals in Fe<Subscript>73.5</Subscript>Si<Subscript>13.5</Subscript>B<Subscript>9</Subscript>Nb<Subscript>3</Subscript>Cu<Subscript>1</Subscript> soft magnetic alloys before and after thermomechanical treatment

The structure of the Fe_73.5Si_13.5B₉Nb₃Cu₁ soft magnetic alloy has been investigated using X-ray diffraction in transmission geometry. The initial alloy prepared by rapid quenching from the melt has a short-range order (∼2 nm) in the atomic arrangement, which is characteristic of the Fe-Si structure with a body-centered cubic lattice. The alloy subjected to annealing contains Fe-Si nanocrystals with sizes as large as 10–12 nm. The annealing under a tensile load leads to an extension of the nanocrystal lattice so that, after cooling, a significant residual deformation is retained. This can be judged from the relative shifts of the (hkl) peaks in the X-ray diffraction patterns measured for two orientations of the scattering vector, namely, parallel and perpendicular to the direction of the load applied. The deformation is anisotropic: within the accuracy of the experiment, no distortions in the [111] direction are observed and the distortions in the [100] direction are maximum. It is known that crystals with a composition close to Fe₃Si exhibit a negative magnetostriction; i.e., their magnetization induced under a load (Villari effect) applied along the [100] direction is perpendicular to this direction along one of the easy magnetization ([010] or [001]) axes. In the alloy, the orientation of the nanocrystal axes is isotropic and the majority of the nanocrystals have a composition close to Fe₃Si. The direction of magnetization of these nanocrystals is determined by the residual deformation of their lattice and lies near the plane perpendicular to the direction of the tensile load applied during heat treatment. This is responsible for the appearance of transverse magnetic anisotropy of the easy-plane type in the Fe_73.5Si_13.5B9Nb₃Cu₁ alloy.     

Microstructure and magnetic properties of Fe72.5Cu1M2V2Si13.5B9 (M=Nb, Mo, (NbMo), (MoW)) nanocrystalline alloys

The microstructure and magnetic properties of Finemet-type Fe_72.5Cu₁M₂V₂Si_13.5B₉ (M=Nb, Mo, (NbMo), (MoW)) alloys have been systematically studied. Results show that the nanocrystalline alloy with M=NbMo has the smallest grain size of about 8 nm. The order of the effect of Nb, Mo and W additions in decreasing the α-Fe grain size in nanocrystalline alloys is Nb>Mo>W. The best DC soft magnetic properties are obtained in the alloy with M=Nb. In the case of AC soft magnetic properties, the Nb alloy also exhibits a very low core loss comparing with typical Finemet alloy. Therefore, the Nb alloy is suitable for use as a transformer core material. In addition, it is shown that a narrow grain size distribution and a uniform dispersion of α-Fe grains in the amorphous matrix are very crucial for the development of new Finemet-type nanocrystalline alloys with good soft magnetic properties.     

FINEMET type alloy without Si: Structural and magnetic properties

Magnetic and structural properties of a Finemet type alloy (Fe_73.5Ge_15.5Nb₃B₇Cu₁) without Si and high Ge content were studied. Amorphous material was obtained by the melt spinning technique and was heat treated at different temperatures for 1 h under high vacuum to induce the nanocrystallization of the sample. The softest magnetic properties were obtained between 673 and 873 K. The role of Ge on the ferromagnetic paramagnetic transition of the as-quenched alloys and its influence on the crystallization process were studied using a calorimetric technique. Mössbauer spectroscopy was employed in the nanocrystallized alloy annealed at 823 K to obtain the composition of the nanocrystals and the amorphous phase fraction. Using this data and magnetic measurements of the as-quenched alloy, the magnetic contribution of nanocrystals to the alloy annealed at 823 K was estimated via a linear model.     

Macroscopic heterogeneity effects in FeNiNbCuBSi ribbons

The effect of Ni substitution on the magnetic response to macroscopic heterogeneity has been investigated on (FeNi)_73.5Nb₃Cu₁B₉Si_13.5 ribbons. 10, 20 and 30 at% of Ni was alloyed to the detriment of Fe. No significant change was observed as to the bias to build heterogeneity in a non-protective annealing ambience. Instead, the favorable insensitivity of magnetic properties to the heterogeneity, as known for the standard Finemet, gets lost with Ni substitution and serious magnetic hardening takes place for higher Ni percentage. These changes are mainly due to the changed intrinsic properties of the Ni-substituted alloys, as high magnetostriction and the occurrence of a Ni-containing phase, if the alloy is nanocrystallized.     

纳米团聚生长的多重分形谱

采用小角x射线散射（SAXS）方法，对两类具有代表性的纳米团聚的生长分形进行了表征.一 类为用化学方法 (水合肼溶液还原法) 制备的纳米金属Ni粉；另一类通过物理方法(纳米晶 化处理)，由非晶基体相中生长纳米晶相、形成非晶/纳米晶双相结构的Finemet (Fe_{73 .5} Cu₁Nb₃Si_13.5B₉) 合金.上述两 类材料的纳米团聚在生长过程中都存在 明显元素扩散迁移，形成在1—100 nm范围内的元素分布非均匀区域.这些元素分布的非均匀 区域具有多重质量生长分形特征，其尺度大小和分布方式对最终的材料的物理性能至关重要 .SAXS方法是表征这类具有分形生长特征的纳米团聚微观结构信息的强有力手段.从方法论的 角度详述了从SAXS测量到获得多重分形谱的处理过程，这一实验研究分析手段对于定量考察 纳米微结构形貌的生长机理和性能的其他研究课题有一定的帮助作用. 关键词： 纳米材料 分形生长 小角x射线散射 磁性材料     

Effect of crystallization annealing under loading on the magnetic properties and the structure of a soft magnetic FeSiNbCuB alloy doped with chromium

The changes of quasi-static magnetic hysteresis loops and X-ray diffraction patterns of the Fe_73.5Si_13.5B₉Nb₃Cu₁ doped to 10 at % chromium instead of iron have been studied to elucidate the influence of the thermomechanical treatment consisting of annealing and cooling of the alloy under the tensile stress (tensile-stress annealing (TSA)) on the magnetic properties and the structure of these alloys. It is shown that the treatment results in the induction of the magnetic anisotropy of the hard axis type at which the magnetization reversal along the direction of applying the external stress during annealing is hampered. The energy of the induced magnetic anisotropy decreases as the chromium content increases. During TSA, the nanocrystal lattices are deformed, and the deformation is retained after cooling. The interplanar spacings increase along the extension direction and decrease in the transverse direction. The deformation anisotropy is observed for crystallographic directions. The anisotropic deformation of the bcc lattice of nanocrystals with high content of the ordered Fe₃Si phase characterized by a negative magnetoelastic interaction is the cause of formation of the state with the transverse magnetic anisotropy of the hard axis type.     

Formation of the nanostructure in amorphous alloys of the Al-Ni-Y system

The formation of the amorphous-nanocrystalline structure during the crystallization of metallic glasses of the Al-Ni-Y system has been investigated by X-ray diffractometry, differential scanning calorimetry, and transmission electron microscopy. It has been shown that the crystallization onset temperature depends on the chemical composition of the alloy, and the crystallization is accompanied by changes in the structure of the amorphous phase, such as the phase separation and the formation of amorphous regions of various compositions with different short-range orders. The nanocrystals nucleate in the amorphous phase by the heterogeneous mechanism. It has been found that the size of precipitated aluminum nanocrystals depends on the alloy composition. The amorphous-nanocrystalline structure formed during the thermal treatment is stable and remains unchanged during the isothermal annealing at 150°C for 500 h.     

Severe plastic deformation of amorphous alloys: I. Structure and mechanical properties

The basic regularities of variation in the structure and mechanical properties of amorphous Ni₄₄Fe₂₉Co₁₅Si₂B₁₀ alloy at severe plastic deformation (SPD) in a Bridgman cell at different temperatures are considered. It is shown that SPD is accompanied by homogeneous nanocrystallization, which is caused by the plastic flow mode. The transition from inhomogeneous mode of plastic flow to a qualitatively different one has been detected. The SPD structural model of deformational “dissolving” of crystals is proposed to explain why nanocrystals no more than 10 nm in size are observed during SPD. It is found that thermally activated nanocrystallization may occur at very low temperatures (77 K) under very high stress and with a high concentration of excess free volume.     

Three-dimensional atomic scale analysis of nanostructured materials

The 3-dimensional atom probe (3DAP) has been used to provide atomic-scale microcharacterisation of a number of nanostructured materials. Grain boundary segregation has been investigated in electrodeposited nanocrystalline nickel and Ni-P. In the nanocrystalline nickel, there was no observable grain boundary segregation in the as-deposited condition. After annealing, carbon and sulphur contamination was found at the boundary of an abnormally-grown grain. In the as-deposited Ni-P alloy, only limited grain boundary segregation of P is seen, but annealing produces significant segregation and the formation of Ni₃P precipitates at grain boundaries. The phase chemistry in a melt-spun amorphous Fe-Si-Cu-Nb-B-Al (FINEMET-type) alloy has also been studied, and the hetereogeneous nucleation of Fe-Si nanocrystals at Cu precipitates shown conclusively. It is found that at early stages of crystallisation, there is only limited partitioning of the Si between the nanocrystals and the amorphous matrix. Atom probe studies of thin layered films have historically been limited by specimen preparation problems, but recent advances have now yielded data on metallic multilayer films. This has allowed atomic-scale measurements of interface chemistry in these films for the first time.     

Structural,magnetic and electrical study of nano-structured α-Fe1.4Ti0.6O3

Nano-structured α-Fe_1.4Ti_0.6O₃ has been synthesized using a simple technique of mechanical alloying. Doping of Ti atoms into α-Fe₂O₃ structure has been characterized by XRD, SEM-EDX, FTIR, VSM and impedance spectroscopy. Magnetic and electrical studies have revealed important changes at the interfaces of grains and grain boundaries, and at rhombohedral planes during formation of α-Fe_1.4Ti_0.6O₃ alloy. The alloy has shown the properties of ferromagnetic semiconductor with substantial increase of magnetic moment and electrical conductivity with the decrease of grain size. The 100 h milled sample has been air annealed to study the effects of thermal activated grain size, lattice structure, magnetism and electrical properties. This work has demonstrated some recent issues of the synthesis of ferromagnetic semiconductor, e.g., structural phase stability, grain size effects, magnetic ordering and electrical conductivity at different stages of the mechanical alloying and subsequent annealing at 700 °C.     

Physical properties and microstructures of nanocrystals reinforced ice laser 3D print layer

Rapid prototyping based on laser alloying by the pre-placed mixed powders has been used to produce the nanocrystals reinforced three-dimensional layer in this study. Such a layer was fabricated on a TC17 titanium alloy by laser rapid prototyping (LRP) of the Co–Sb–TiB₂ mixed powders in ice. Scanning electron microscope (SEM) and high resolution transmission electron microscopy (HRTEM) test results indicated that the ice addition was able to decrease the maximum temperature of molten pool during the LRP process, favoring the formation of nanocrystals; growth of such nanocrystals was retarded by the surrounded amorphous in a certain extent, favoring the formations of ultrafine nanoparticles (UN), and the twin crystals and the high-angle grain boundaries were also observed; differential thermal analysis (DTA) test was used to explain the physical properties and formation mechanism of amorphous–nanocrystals, and also the relationship between the amorphous and nanocrystalline phases in such a LRP layer.     

Metastable phases in vapour-quenched Al78Cu22 film

The structure and structural changes of an Al₇₈Cu₂₂ (at%) alloy film produced by coevaporation onto a cooled substrate have been investigated with transmission electron microscopy. A series of metastable phase transitions were observed during the crystallization from the as-deposited amorphous phase to the final equilibrium state. The deposit structure at room temperature consists of a mixture of fine grained α' crystallites (fcc, α = 4.81 Å) with an amorphous phase, and some welldefined crystals with an fcc lattice (a = 7.18 Å, namely α₁). The subsequent annealing led to the grown crystals transforming to an ordered α′ phase. It is argued that the development of such a transition is the result of a gradual atomic rearrangement – first topologically then a chemically predominant disorder-order transition.     

The existence of giant magnetocaloric effect and laminar structure in Fe73.5−xCrxSi13.5B9Nb3Cu1

Amorphous soft magnetic ribbons Fe_73.5−xCr_xSi_13.5B₉Nb₃Cu₁ (x=1–5) have been fabricated by rapid quenching on a single copper wheel. The differential scanning calorimetry (DSC) patterns showed that the crystallization temperature of α-Fe(Si) phase is ranging from 542 to 569 °C, a little higher than that of pure Finemet (x=0). With the same annealing regime, the crystallization volume fraction as well as the particle size of α-Fe(Si) crystallites decreased with increasing Cr amount substituted for Fe in studied samples. Especially, the interesting fact is that the laminar structure of heat-treated ribbons on the surface contacted to copper wheel in the fabricating process has been firstly discovered and explained to be related to the existence of Cr in studied samples. The hysteresis loop measurement indicated that there is the pinning of displacement of domain walls. The giant magnetocaloric effect (GMCE) has been found in amorphous state of the samples. After annealing, the soft magnetic properties of investigated nanocomposite materials are desirably improved.     

Structural and technical details of the Kirkwood-Buff integrals from the optimization of ionic force fields: focus on fluorides

Polymer crystals are metastable and exhibit morphological changes when being annealed. To observe morphological changes on molecular scales we started from small nanometer-sized crystals of highly folded long-chain polymers. Micron-sized stripes consisting of monolayers or stacks of several layers of flat-on oriented polyethylene nanocrystals were generated via evaporative dewetting from an aqueous dispersion. We followed the morphological changes in time and at progressively higher annealing temperatures by determining the topography and viscoelastic properties of such assemblies of nanocrystals using atomic force microscopy. Due to smallness and high surface-to-volume ratio of the nanocrystals, already at 75 °C, i.e. about 60 degrees below the nominal melting point, the lateral size of the crystal coarsened. Intriguingly, this occurred without a noticeable reduction in the number of folds per polymer chain. Starting at around 110 °C, chain folds were progressively removed leading to crystal thickening. At higher temperatures, but still below the melting point, prolonged annealing allowed for surface diffusion of molten polymers on the initially bare substrate, leading eventually to the disappearance of crystals. We compared these results to the behavior of the same nanocrystals annealed in an aqueous dispersion and to bulk samples.     

The rapid preparation of large-scale CdS opal photonic crystals and study of the optical properties

Monodispersed silica microspheres of 270 nm are synthesized by a colloidal solution method. Larger scale perfect three-dimensional photonic crystals (PCs) are rapidly prepared using the evaporation of acetone to self-assemble the microspheres on quartz substrates by vertical deposition methods. We find that the pseudo-photonic band gap (PBG) of the PC structure changes with increasing annealing temperature; it drastically shifts from 450 nm for as-grown crystals to 409 nm for annealing at 800 °C. CdS photonic crystals are formed by infiltrating CdS nanocrystals of 6 nm into the SiO₂ PC structure. The transmission and spontaneous emission characteristics of CdS PCs have been investigated. The clear dip in the spontaneous emission spectrum relates to the photonic band gap of CdS PCs, indicating that the spontaneous emission is inhibited in the region of the PBG. The emission band of CdS PCs becomes narrower and sharper than that of CdS nanocrystals; this demonstrates that the emission band and intensity of the luminescent devices will be tuned by controlling the position of the PBG. PACS 42.70.Qs; 42.25.Bs; 78.20.-e; 78.55.Et     

The effect of hardening by annealing in ultrafine-grained Al–0.4Zr alloy: influence of Zr microadditives

Influence of annealing on the microstructure and mechanical properties has been studied for Al–Zr (0.4 wt.%) alloy with the ultrafine-grained (UFG) structure formed by high-pressure torsion (HPT) at room temperature. A drastic hardening effect by short-term annealing in the temperature range of 90–280°С was observed for the HPT-processed Al–Zr alloy. The effect of hardening by annealing for the HPT-processed Al–Zr alloy is compared with that for the HPT-processed commercial purity (CP) Al. It was shown that addition of 0.4 wt.% Zr in Al does not cause a significant impact on the magnitude of hardening by annealing up to 150°С, however it leads to a shift of its maximum to higher annealing temperatures and expansion of the thermal stability range of strength up to 280°С. The kinetics of hardening by annealing for CP Al and Al–Zr alloys in the UFG state has been studied for the first time. It was shown that in both materials the strength first increases linearly with the duration of annealing and then reaches saturation. The temperature dependence of the rate of hardening by annealing was analysed through an Arrhenius law, and apparent activation energy was extracted for both systems. The addition of Zr results in the reduction of the activation energy of annealing-induced hardening by ～2 times. Possible physical mechanisms controlling the kinetics of hardening by annealing are discussed for the ultrafine-grained CP Al and Al–Zr alloy.     

Effect of nonstoichiometry on the plastic behavior of Ni<Subscript>3</Subscript>Ge single crystals with the [001] orientation of the deformation axis

The effect of nonstoichiometry on the mechanical properties of Ni₃Ge alloy single crystals with the [001] orientation of the deformation axis has been investigated. It is shown that the limits of the temperature range of different stages shift to higher temperatures with an increase in nonstoichiometry. A change in the alloy composition only slightly affects the temperature dependence of the work hardening rate.