Study of nanocrystalline Fe－Al－N soft magnetic thin films

Fe－Al－N films were fabricated by reactive sputtering using a radio-frequency magnetron sputtering system. The effects of Al and N content and annealing temperature on microstructure and magnetic properties were investigated. The Fe－Al－N films, which have good soft magnetic properties, consist of nanocrystalline α-Fe grains and a small amount of other phases in the boundaries of α-Fe grains. The average α-Fe grain size is about 10－15nm. A slight amount of Fe－N and Al－N compounds precipitate in the boundaries of α-Fe grains and suppress their growth. Annealing improves the soft magnetic properties slightly by releasing the residual stress and reducing defects.     

铝基非晶合金微观结构的特点与演变

选择Al90Fe5Ce5和Al83Zn7Ce10非晶合金来研究铝基非晶合金的微观结构的特点和微观结构的演变.在Al90Fe5Ce5非晶合金中,发现亚稳Al6Fe相与被铝相包裹的二十面体准晶相共存.在Al83Zn7Ce10非晶合金中,金属间化合物Al2ZnCe2为凝固过程中的初生相.金属间化合物Al2ZnCe2可以伴随纳米晶粒铝的晶化而析出.抑制在冷却过程中所形成的各种晶核的成长是铝基合金具有很强的非晶形成能力的主要原因.多种相的竞争形核和有限生长导致了铝基合金具有复杂的结构特点 关键词： 铝基非晶合金 二十面体准晶 预峰 化学短程序     

Investigation of magnetic properties in 57Fe/Al multilayers

Fe/Al multilayer thin films prepared by ion beam sputtering, with an overall atomic concentration ratio of Fe/Al = 1:2 have been studied by x-ray diffraction spectroscopy (XRD), X-ray reflectivity (XRR) and D.C. Magnetization. These studies show the formation of Fe–Al intermetallic layers. Two magnetic regions and transition temperatures of 473 and 533 K are evident from magnetization studies. Conversion Electron Mössbauer Spectroscopy (CEMS) shows formation of off-stoichiometric Fe₃Al like phase and phases consisting of pure Fe and Fe-rich extended Fe–Al solutions.     

Magnetic properties of nano-sized 5 at.%Fe–Al systems

High energy ball milling is a promising materials processing technique that is widely used to produce nanocrystalline structures. However, when stainless steel or hardened steel containers and balls are used for milling, contamination from the milling medium can influence the material properties of the final nanostructured products due to intercalation of iron (Fe) as an impurity. This study reports the effect of iron contamination on nanocrystalline aluminum (Al) powder. ⁵⁷Fe Mössbauer spectroscopy and bulk magnetization studies using a vibrating sample magnetometer show that pure Al powder milled in hard steel media is strongly ferromagnetic at room temperature due to Fe contamination of about 5 at.% from the milling medium. TEM studies indicate that the system consists mainly of nano-sized Fe interspersed in Al with average crystallite sizes of ~2 and ~5 nm for Fe and Al, respectively. A comparative study of this system made with a mechanically alloyed Fe–Al system with the same percentage of Fe mixed with pure Al and mechanically alloyed using tungsten carbide vials and balls shows that the saturation magnetization, coercivity, Curie temperature, and low temperature behavior (field cooled–zero field cooled) are very different in the two cases. The different magnetic properties of the two systems can be attributed to the presence of magnetic and non-magnetic phases present.     

PLD方法制备的纳米Fe/Al薄膜的结构及应力分析

 采用PLD方法制备了Fe/Al合金薄膜，研究了Fe/Al合金薄膜的物相、结构、应力等。研究表明薄膜的沉积速率随着衬底温度的升高而降低。原子力显微镜（AFM）图像显示，薄膜表面平整、致密且光滑，均方根粗糙度小于1 nm。等离子体发射谱（ICP）表明Fe/Al原子比为1∶1。X射线小角衍射（XRD）分析表明薄膜中的物相是Al_0.5Fe_0.5，Al_0.5Fe_0.5晶体具有简单立方结构(SC)，晶格常数为0.297 nm，平均晶粒尺寸为81.74 nm，平均微畸变为0.007 6。     

High-intensity ion implantation - a technique to form finely dispersed intermetallic compounds in surface layers of metals

The results of experimental investigations of microstructure and phase composition of surface ion-alloyed layers of nickel, titanium, and iron formed under the conditions of high-intensity aluminum-ion implantation are presented. It is established that aluminum-ion implantation under high-intensity modes makes it possible to form finely-dispersed intermetallic phases of Me₃Al (Me = Ni, Ti, Fe) and MeAl (Ni, Ti), as well as solid solutions of a composition variable with respect to depth in the surface layers measuring up to 2000 nm. It is shown that the average grain-size of intermetallic phases formed in ion-alloyed layers is 20–80 nm. Regions of localization of the phases thus formed over the implanted layer depth are determined.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 9, pp. 44–52, September 2004.     

Effect of Xe ion irration of Fe/Sn bilayers

Films of Fe (20 nm) and Sn (40 nm) have been deposited by PVD onto Al supports and irradiated with 100 keV Xe ions at a dose of 5×10¹⁵ ions/cm². Scanning electron microscopy (SEM) shows that the irregular morphology of deposited Sn is considerably flattened by irradiation, which produces also a noticeable sputtering of Sn. Conversion electron Mössbauer spectroscopy (CEMS) reveals the formation at the interface of a variety of intermetallic phases which is enhanced by irradiation. These phases, seem to be insensible to prolonged (several months) room temperature aging. Their thermal stability under annealing at temperature up to 523 K has also been investigated.     

Fe/Al混合膜的PLD法制备及表面分析

 采用脉冲激光气相沉积（PLD）技术制备了Fe/Al混合膜，测量了该混合膜的光电子能谱（XPS），并采用原子力显微镜（AFM）、扫描电子显微镜（SEM）对Fe/Al混合膜作了表面分析。结果表明：Fe/Al混合膜的表面粗糙度对衬底温度有明显的依赖性， 随着衬底温度的升高，薄膜的表面逐渐变得平滑，膜层变得致密，在200 ℃衬底温度下制得了均方根（rms）粗糙度为0.154 nm、具有原子尺度光滑性的Fe/Al混合膜， 膜中Fe和Al分布比较均匀，其成分比约为1∶3，同时XPS分析也表明Fe/Al混合膜暴露在空气中后表面形成了Al₂O₃和FeO氧化层。     

Transmission electron microscopy and X-ray diffraction study of microstructural evolution in magnetoresistive Cu–Fe–Ni ribbons

The evolution of the microstructure of a granular Cu₈₀Fe₁₀Ni₁₀ (at%) melt-spun ribbon is studied by transmission electron microscopy (TEM), energy-filtered transmission electron microscopy (EFTEM) and X-ray diffraction. This system is interesting as large giant magnetoresistance (GMR) values have been measured for this composition. We have shown the presence of two face-centred cubic phases, an (Fe,Ni)-rich phase and a Cu-rich phase. The lattice parameters of these two phases are close and no diffraction or elastic contrast is involved in displaying the two phases in TEM bright-field mode. With EFTEM imaging, we have shown the presence of a fine-scale (Fe,Ni)-rich precipitation inside the Cu-rich fcc matrix. The precipitates are 2–4 nm in the as-spun state and 4–6 nm after annealing for 2 h at 400°C. The lattice parameter of the Cu-rich phase in the as-spun sample is 0.3608 nm and 0.3610 nm for the (Fe,Ni)-rich phase. After a 24-h annealing treatment at 600°C, the mean diameter of the particle is 20 nm and the lattice parameter of the (Fe,Ni)-rich phase has decreased to 0.3600 nm, while that of the Cu-rich phase has increased to 0.3613 nm, which is consistent with a segregation of Fe and Ni in the precipitates. The composition and volume fraction of the two phases measured for this annealed sample are in good agreement with the Thermocalc® predictions.     

The use of macroscopic modelling of intermetallic phases in aluminium alloys in the study of ferricyanide accelerated chromate conversion coatings

Chromate conversion coatings are used on aluminium alloys, primarily for their renowned corrosion resistant properties. Although these coatings are in common industrial use, neither the protection mechanisms, nor the coating interation with the intermetallic precipitation phases are fully understood. Macroscopic models have been developed in order to represent the galvanic cells present in aluminium alloys due to the presence of such intermetallic particles. Particles modelled include CuAl₂, FeAl₃ and Cu₂FeAl₇, all know to be cathodic to the aluminium matrix. Variations in deposition, both in composition and thickness, are indicative of the mechanisms of deposition over each phase. Characterisation of the coating deposition was carried out using X-ray photoelectron spectroscopy, Rutherford backscattering spectroscopy, Auger electron spectroscopy, scanning electron microscopy with X-ray analysis. Depositional characteristics have been determined for each phase. The coating on the intermetallic phases is primarily Al oxide, and is significantly thinner than the coating on the matrix. This coating on the matrix consists mainly of a mixed Cr/Al oxide. The coating on the intermetallic phases was only one tenth the thickness of the matrix coating, and contained higher levels of Fe, Al and O. Matrix coating chemistry predominated with Cr, O, Fe and N, indicative of a chromate conversion coating. The mechanism for reduced rates of deposition over intermetallic phases was found to be affected by fluorine ion attack leading to intermetallic de-alloying and decomposition of Fe(CN)₆²⁻ accelerator into amide groups on the matrix.     

Microstructure characterization of Al matrix composite reinforced with Ti-6Al-4V meshes after compression by scanning electron microscope and transmission electron microscope

Compressive properties of Al matrix composite reinforced with Ti-6Al-4V meshes (TC4(m)/5A06 Al composite) under the strain rates of 10(-3)S(-1) and 1S(-1) at different temperature were measured and microstructure of composites after compression was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Compressive strength decreased with the test temperature increased and the strain-rate sensitivity (R) of composite increased with the increasing temperature. SEM observations showed that grains of Al matrix were elongated severely along 45° direction (angle between axis direction and fracture surface) and TC4 fibres were sheared into several parts in composite compressed under the strain rate of 10(-3)S(-1) at 25°C and 250°C. Besides, amounts of cracks were produced at the interfacial layer between TC4 fibre and Al matrix and in (Fe, Mn)Al(6) phases. With the compressive temperature increasing to 400°C, there was no damage at the interfacial layer between TC4 fibre and Al matrix and in (Fe, Mn)Al(6) phases, while equiaxed recrystal grains with sizes about 10 μm at the original grain boundaries of Al matrix were observed. However, interface separation of TC4 fibres and Al matrix occurred in composite compressed under the strain rate of 1S(-1) at 250°C and 400°C. With the compressive temperature increasing from 25°C to 100°C under the strain rate of 10(-3) S(-1), TEM microstructure in Al matrix exhibited high density dislocations and slipping bands (25°C), polygonized dislocations and dynamic recovery (100°C), equiaxed recrystals with sizes below 500 μm (250°C) and growth of equiaxed recrystals (400°C), respectively.     

聚合氯化铝铁溶液的可见光谱与碱化度、总铁浓度关系研究

研究了不同碱化度Ｂ、不同铝铁摩尔比的聚合氯化铝铁（ＰＡＦＣ）溶液的可见光谱。发现它们在４６０ｎｍ波长处吸光度Ａ与溶液的碱化度Ｂ线性相关;用该波长处吸光度Ａ对铝铁摩尔比作图出现的折点与它们的ｐＨ－ｎＡｌ／ｎＦｅ（铝铁摩尔比）曲线上ｐＨ突跃点正好对应。说明这些折点分别代表了不同Ｂ值下溶液中配体ＯＨ＾－在Ｆｅ（Ⅲ）与Ａｌ（Ⅲ）羟基配合物间的平衡配比。由此找出了ＰＡＦＣ溶液的碱化度Ｂ、总铁浓度〔Ｆｅ〕Ｔ与     

Effect of thin aluminum interlayer on growth and microstructure of carbon nanotubes

The aluminum (Al) interlayer with various thicknesses ranging from 0.75 to 6 nm was deposited on silicon (Si) substrates prior to the deposition of ultra-thin iron (Fe) catalyst for the growth of carbon nanotubes. In this paper we report the effect of ultra-thin Al interlayer on the growth of multiwalled carbon nanotubes (MWCNTs). The SEM was used to examine the microstructures of nanotubes. We observed as the Al interlayer thickness increases the height of nanotube decreases. Raman spectra of MWCNT showed typical D and G peaks at ∼1345 cm⁻¹ and ∼1575 cm⁻¹, respectively. The XPS revealed the presence of Al and Fe on the top of CNT surface which were further supported by TEM. The high resolution TEM results also revealed bamboo like CNTs with diameter ∼10–40 nm.     

Reaction mechanisms between Al and Fe3O4 powders in the formation of an Al-based metal matrix composite

The reaction mechanisms between Al and Fe₃O₄ powders were investigated. Differential thermal analysis revealed that a two-step displacement reaction between Al and Fe₃O₄ took place during sintering. Initially, the Fe₃O₄ was converted to amorphous FeO at ～720°C and some of the Al was oxidized to amorphous Al₂O₃. In the final stage, when the temperature reached ～840°C, crystalline Al₂O₃ particles were produced in the molten Al–Fe liquid. The effects of cooling rate on the microstructures were studied. When the Al–Fe liquid was furnace-cooled to room temperature, proeutectic Al₃Fe plates, plate-like divorced eutectic Al₃Fe and Al₂O₃ particles were in situ formed in the Al(Fe) matrix. While quenching from 700°C, nanometer-sized Al dendrites and Al–Al₆Fe eutectic lamellae were produced in the Al matrix. However, when it was rapidly quenched from 900°C, the size of the proeutectic Al₃Fe phases was further reduced and Al₆Fe nanorods were found in the Al–Al₆Fe eutectics. A model was proposed to describe the transformation of the Al–Fe intermetallics during solidification.     

微合金化元素对Fe-Al界面结合的第一性原理研究

利用第一性原理中的DFT理论研究了Fe/Al界面的能量学和电子结构,讨论了替位型掺杂的元素Zn、Mn、Ni在Fe/Al界面处的作用.结果表明:元素Zn、Mn、Ni都会优先替换界面处的Fe原子,使得界面结合能增加,体系更稳定,有利于界面的结合;跨界面的Fe原子与Al原子之间的电荷布居、键长以及差分电荷密度图的计算表明:掺杂后有利于跨界面的Fe-Al间成键,从而加强了Al层与Fe基体的结合,且结合强度由强到弱依次为:掺Zn>掺Mn>掺Ni;与实验比较吻合.最后对掺杂Zn的增韧机理加以解释.     

Microstructural characterization of rapidly solidified Al 90 Ce 10 alloy

In the present work, the microstructure of the melt-spun Al 90 Ce 10 alloy has been characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM) together with energy-dispersive spectrometry. It has been found that the microstructure of the melt-spun Al 90 Ce 10 alloy is composed of the amorphous phase, f-Al, f-Al 11 Ce 3 , Al 3 Ce and unidentified phases, quite different from that of the ingot-like alloy consisting of coarse primary f-Al- f-Al 11 Ce 3 dendrites embedded in the f-Al- f-Al 11 Ce 3 eutectic matrix. Moreover, the amorphous phase is dominant in the melt-spun Al 90 Ce 10 alloy according to the XRD and TEM results. Al 3 Ce particles, less than 100 nm in size, are dispersed in the partial amorphous phase. Polygonal f-Al 11 Ce 3 crystals embedded in the f-Al matrix are also observed. The presence of the hexagonal, kite-like and petal-like intermetallic particles surrounded by the amorphous phase indicates that there exist micro-inhomogeneous structures in the Al 90 Ce 10 melt. These results demonstrate that the overheating of the melt has a significant effect on the amorphization of the Al 90 Ce 10 alloy.     

Study of thickness-dependent magnetic and transport properties of Fe/Al nanostructures

The paper presents magnetic and transport properties of compositionally modulated Fe/Al multilayer structures (MLS), with an overall atomic concentration ratio of Fe:Al = 3:1, 2:1 and 1:1. All MLS show soft ferromagnetic behaviour at room temperature (RT) with an in-plane easy axis of magnetization. In each case, coercivity increases continuously and magnetization decreases with an increase in temperature due to enhancement in the anisotropy as a result of non-uniform and disordered formation of thin intermixed (dead) FeAl layer at the interfaces. The Curie temperature obtained for the MLS is much less than that of bcc Fe but is well above RT. The observed magnetic behaviour is mainly attributed to the formation of different FeAl phases and increase in anti-ferromagnetic interlayer coupling with addition of Al. The formation of these phases is also supported by resistivity results. The results of this research enabled us to understand that by controlling of layers thickness and temperature in multilayer systems, the nanogranular thin films with good resistive and soft magnetic properties can be obtained.     

通过插入Au薄膜改善绿光OLED器件的发光色纯度

在一些有机电致发光器件中,Au常被用作阳极,研究者希望Au在导电的同时兼具半透明可出光的属性,这要求Au在能导电的同时厚度要尽量薄。因此制备两种金属共同组成电极成为了选择。将半透明Au/Al层插入阳极一侧,制备了结构为ITO/Al(16 nm)/Au(10 nm)/TPD(30 nm)/AlQ(30 nm)/LiF(0.5 nm)/Al的OLED器件,相对于器件ITO/TPD(30 nm)/AlQ(30 nm)/LiF(0.5 nm)/Al在长波方向出现了光谱窄化现象,通过分析和实验判断该现象是Au薄膜特有的对光的选择透过性造成,而并非微腔效应。阳极一侧加入了Au/Al的器件保持了广视角无角度依赖的优点,同时可以输出滤掉部分红光的纯度更高的发光,发光色纯度得到了改善。     

Thickness dependence of the magnetic anisotropy of Fe layers separated by Al

Magnetic multilayers of ⁵⁷Fe with nominal thickness, T _nom, between 0.4 and 1.0 nm separated by 3.0 nm Al spacer layers were prepared by alternate deposition of the constituents in high vacuum. The samples were investigated at 4.2 K in external magnetic field. A fraction of Fe atoms corresponding to about 0.3 nm equivalent Fe-thickness was found to mix into the Al spacer. The extremely strong magnetic anisotropy observed for T _nom < 0.8 nm is attributed to Fe layers of approximately two atomic planes thick. The anisotropy decreases considerably after the building up of the third Fe atomic layer starts at T _nom = 0.8 nm, but full saturation was not achieved even for T _nom = 1 nm and 3 T magnetic field applied perpendicularly to the sample plane.     

Role of precursor alloy phases and intermediate oxides in the preparation of Raney and Urushibara iron

⁵⁷Fe Mössbauer spectroscopy and scanning electron microscopy measurements of precursor phases formed during catalyst preparation and of the catalysts, themselves, demonstrate that the preparation of Raney iron from iron aluminum alloys involves the formation of Fe(OH)₂ and Fe₃O₄ as intermediate phases. The metallic Fe is formed from subsequent reduction of Fe₃O₄ by hydrogen generated by the oxidation of aluminum metal by hydroxide ions. Precursors to Urushibara iron U?Fe (III) are found to consist of Fe?Zn alloys when Zn is used as a reductant and of epitaxial deposits of Fe on aluminum when Al is the reductant. The material resulting from the reduction of the iron salt by aluminum is not a hydrogenation catalyst; the absence of catalytic activity is related to the absence of any alloying of the iron and aluminum. A consideration of the preparation of Raney iron, Urushibara iron, ammonia synthesis and Fischer-Tropsch catalysts leads to the conclusions that catalytic activity is highly correlated to the existence of intermediate mixed-crystals phases and the presence of intimate mixtures of at least two phases in the final catalyst.