Crystallization of cobalt amorphous alloys under field annealing

Crystallization of Co-rich amorphous ribbons annealed under a 10 Oe external magnetic field at the early 30 minutes from their glassy status to supercooled liquid status is investigated by high-resolution transmission microscope (HR-TEM), Selected Area Fourier Transform (SA-FT), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicate that the short-rang ordering feature can be refined very well in specimen annealed under temperatures about 87.4 degrees C below their glass transition (Tg), showing refined salt-pepper morphologies with a mean length changing from 1.2 +/- 0.8 nm to 0.8 +/- 0.2 nm and a mean width shifting from 0.5 +/- 0.2 nm to 0.3 +/- 0.1 nm. When the amorphous ribbons are field-annealed at temperature near to Tg (i.e., 450 degrees C), ultra-fine nanocrystalline structures can be formed on the top surface of ribbons with size of 3.5 +/- 0.5 nm and inter-grain spacing of about 0.4 +/- 0.2 nm even though the inner parts of the ribbons are still in amorphous phases. The nanocrystalline areas are featured by the formation of doped hcp cobalt phase orientated along the c-axis, with the inter-plane spacing ranging from 4 A to 6 A. When the annealing temperature is above Tg, the grain sizes are increased dramatically with multi-phased nanocrystals precipitating from the amorphous substrate, and finally reaching almost complete crystallization at 600 degrees C, causing greatly coarsening of the nanocrystal structures.     

热处理对(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶合金的组织结构及磁性能的影响

采用单辊急冷法制备(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶薄带,并对该合金进行等温退火。采用XRD,AFM,VSM研究退火温度对(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶合金的组织结构和磁性能的影响。结果表明:非晶合金晶化过程为Am→α-Fe(Co)+Am′→α-Fe(Co)+Cr_2Ni_3+Fe_3Ni_2+Cr_2Zr+未知相。当退火温度Ti玻璃转变温度Tg时,由于结构弛豫、内应力的释放,合金的饱和磁化强度Ms有所提高;当晶化起始温度TxTi第一晶化峰值温度Tp1时,由于铁磁性α-Fe(Co)相的析出,Ms显著提升;当TiTp1时,由于晶粒长大和第二相的析出,Ms急剧恶化,565℃退火能够获得最好磁性能(Ms=106.8A·m~2·kg~(-1))。490℃和565℃退火后薄带表面的AFM观察表明,AFM图片所呈现的颗粒尺寸要比用Scherrer法测得的α-Fe(Co)纳米晶尺寸大得多,这是典型的包裹晶粒现象。     

Structural and Mössbauer effect investigations of amorphous FeCuNbSiB alloys nanocrystallized (VITROPERM) in magnetic field

Melt-spun amorphous ribbons of nominal composition Fe73Cu1Nb3Si16B7, annealed at 560-580 degrees C for 1 hour in a magnetic field (H) applied along the width in the ribbon plane, develop uniaxial magnetic anisotropy with easy axis along H and exhibit several novel attributes. The samples labelled as S20 and S150 are nanocomposites consisting of ferromagnetic nanocrystalline grains (volume fraction approximately equal to 84% and 81%) of mean size d = 13(2) nm embedded in a ferromagnetic amorphous matrix and possess a magnetic permeability as large as 20,000 and 150,000, respectively. While nearly 55% of the nanocrystalline grains have a cubic DO3 Fe3Si-like structure with actual Si concentration of about 22 at.%, the remaining 45% nanocrystalline grains have tetragonal Fe3B and hexagonal Fe2Si structure. Since the crystalline volume fraction of Fe3B and Fe2Si nanocrystals is more in the sample S20, this sample exhibits stronger local magnetic anisotropy and hence lower permeability.     

Corrosion behaviors of amorphous and nanocrystalline Fe-based alloys in NaCl solution

Amorphous Fe(73.5)Si(13.5)B9Nb3Cu1 alloy was prepared by the chill block melt-spinning process and nanocrystalline Fe(73.5)Si(13.5)B9Nb3Cu1 alloy was obtained by annealing. The crystallization behaviors were analysed by DSC, XRD and TEM. The electrochemical corrosion behaviors in different annealed states were performed by linear polarization method and electrochemical impedance spectroscopy in 3.5% NaCl solution. The results show that the crystallization of amorphous alloy occurs in the two steps. Some nanometer crystals appear when annealing in 550 degrees C and 600 degrees C, respectively with grain size 13 nm and 15 nm. The nanocrystalline alloy has a tendency to passivation and lower anodic current density than amorphous alloy. It indicates that nanocrystalline alloy has a higher corrosion resistance. Amorphous Fe(73.5)Si(13.5)B9Nb3Cu1 alloy consisted of only single semi-circle. When the alloy was annealed in 600 degrees C, its EIS consisted of two time constants, i.e., high frequency and low frequency capacitive loops. The charge transfer reaction resistances increases as annealing temperature rises.     

Enhancement of the giant magnetoimpedance effect and its magnetic response in ion-irradiated magnetic amorphous ribbons

The influences of N and Xe ion irradiation on the giant magnetoimpedance (GMI) effect and its magnetic response in Co₆₉Fe_4.5Al_1.5Si₁₀B₁₅ amorphous ribbons were systematically investigated. A large enhancement of the GMI effect and its magnetic response were achieved in N and Xe ion-irradiated amorphous ribbons. At a frequency of 3 MHz, the GMI ratio and magnetic response for an N-ion-irradiated amorphous ribbon respectively reached the highest values of 130% and 13%/Oe, while for a non-irradiated amorphous ribbon they were only about 53% and 8%/Oe. The enhancement of the GMI effect and magnetic response in the ion-irradiated amorphous ribbons resulted from the enhancement of the permeability due to rotational magnetization. Our studies indicate that low energy ion irradiation is useful for improving the magnetic softness, GMI and magnetic response of amorphous alloys, which is of practical importance for the development of high-performance magnetic sensors.     

Giant Magnetoimpedance Current Sensor With Spiral Structure Double-Probe

A novel giant magnetoimpedance (GMI) noncontact current sensor with spiral structure double-probe is designed. Differing from the formerly reported sensors, the probes of this sensor consist of annealed commercial amorphous ribbons which are curled to spiral tubes. Two couples of permanent magnets are applied to provide bias magnetic field. The distance between the probes and the permanent magnets is fixed at 2.4 cm. The sensor shows sensitivity of 1 V/A in the current range of $pm$ 1.5 A, measurement precision of less than 0.16% at room temperature, and good thermal stability in the temperature range between $-$20 and 30 $;^{circ}{rm C}$.      

Structure and Magnetic Properties of Fe_(76.5)Si_(13.5)B_9Cu_1 Alloy with Nanoscale Grain Size

The structure and magnetic properties of Fe76.5Si13.5B9Cu1 alloys with a nanocrystalline (NC) bcc Fe(Si) phase trom about 23 to 46 nm in diameter, which were first formed into amorphous ribbons and then annealed at various temperatures between 703 and 773 K, have been investigated. At annealing temperatures from 703 to 748 K, the single NC bcc(Si) phase is obtained in the crystallized alloys. The grain size and the Si-content in the NC bcc Fe(Si) phase for the alloys annealed at different temperatures are presented. The soft magnetic properties and the saturation magnetostriction for the alloys with the NC bcc Fe(Si) phase are also measured. The results show that, the saturation magnetizotion and the permeability are improved for the alloys with only the NC bcc Fe(Si) phase and become better with decreasing of the NC bcc phase size, and the saturation magnetostriction declines for the alloys with increasing Si-content in the NC bcc Fe(Si) phase.     

Effect of the current annealing (without and with tensile stress) on the soft magnetic behaviour of Fe73.5-x(Co0.5Ni0.5)xSi13.5B9Nb3Cu1 alloy ribbons (x = 2.5, 5 and 10)

Experimental data on microstructural (crystalline volume fraction, grain size) and magnetic (coercive field) properties in amorphous and nanocrystalline Fe73.5-x(Co0.5Ni0.5)xSi13.5B9Nb3Cu1 alloy ribbons (x = 2.5, 5 and 10) are presented. Nanocrystalline structure was developed by annealing the precursor amorphous ribbons by current annealing (CA) and stress-current-annealing (SA). Microstructural analysis of the treated ribbons using X-ray Diffraction showed a high content of amorphous phase in the bulk. In addition, substantial changes in the crystalline state such as grain size of the samples annealed at different conditions were observed. The alloy composition also affects greatly the grain size,: increasing the (Co,Ni) content leads to higher values of the average grain size. The evolutions of the coercive field with the two kinds of thermal treatment were analysed, allowing us to conclude that the addition of (Co,Ni) tends to reduce the magnetic softness character of the original material, while the treated SA samples show higher coercivities higher than those treated without by CA.     

制备态(Fe88Zr7B5)100-xCux非晶薄膜的磁特性和巨磁阻抗

采用射频溅射法在单晶Si衬底上制备了Fe88Zr7B5)100-xCux(x=0、1、2、3、4)非晶薄膜样品,对其软磁特性和巨磁阻抗(GMI)变化行为进行了测量和研究。测量结果显示,加入适量Cu元素(x=3)的制备态样品具有极好的软磁性能和GMI效应,此样品的矫顽力仅有56A/m,在13MHz的频率下,最大有效磁导率(μe)比和GMI比分别为42.5%和17.0%。研究发现,制备态样品的电阻R、电抗X和阻抗Z都随Cu含量的增加而下降。X=0、4两个样品的μe、R、X、Z对外加磁场响应极不敏感,只有软磁性能优异的x=3样品的μe、R、X、Z才显示出对外加磁场响应敏感,因而有显著的GMI效应。样品拥有高的磁导率、小的矫顽力和低的电阻率是获得大GMI效应的本质条件。     

Nanocrystalline Hf and Ta containing FeCo based alloys for high frequency applications

FeCo based nanocrystalline materials have excellent soft magnetic properties even at high temperature, but are limited to low frequency applications due to their relatively low electrical resistivities, ρ_e, resulting in high eddy current losses. Amorphous alloys of (Fe₈₁Co₁₉)₈₄M₉B₇ where M = (Hf, HfTa, Ta) were prepared by meltspinning and annealed for increasing times at their respective crystallization temperatures. The nanocrystalline alloys had coercivities less than 0.4 Oe and saturation inductions greater than 1 T. The electrical resistivities of the amorphous ribbons were all similar with values of ρ_e ? 180 μΩ cm. After annealing at the crystallization temperature, the M = Ta alloy had the largest ρ_e of 140 ± 3 μΩ cm. The Ta alloy also had the best high frequency properties, with an initial permeability of 822 at 1 MHz.     

Characterization of Amorphous GMI Thin-Film Meander Trilayers

This paper presents the magnetic properties of CoFeB trilayer thin films in relation to the high-frequency impedance responses. Fifty- and 100-nm-thin amorphous layers with a central 100- and 200-nm-thin Cu layer, respectively, were sputtered onto a thermally oxidized Si wafer. 300-$muhboxm$-long meanders of 3–20-$muhboxm$width were structured using a standard mask with various meanders, which were connected in series and were then formed by plasma etching. Magnetization curves, parallel to the easy axis, and hard axis of uniaxial anisotropy, were measured by the magnetoptical Kerr effect exhibiting anisotropy fields of around 2 kA/m and low coercivity in the hard-axis direction, depending on the film thickness. The magnetoimpedance (MI) effect was measured manually from 10 MHz to 1 GHz by means of a network analyzer using the reflected wave through the sample. The maximum effect occurred for both samples at 850 MHz.     

Co-Finemet非晶合金晶化动力学及其纳米晶粉芯的磁性

利用单辊熔体快淬法在大气环境中制备了Fe73.5-xCoxSi13.5B9Cu1Nb3(x=10,30,50)非晶薄带,利用差示扫描量热法(DSC)研究了非晶薄带的晶化动力学行为。采用Kissinger和Ozawa方法计算了非晶薄带的晶化表观激活能,计算结果表明:随着Co含量的增加,一次晶化的表观激活能降低而二次晶化的表观激活能升高。利用Johnson-Mehl-Avrami(JMA)模型计算了非晶薄带一次晶化的局域Avrami指数m,计算结果表明非晶薄带一次晶化的机理在不同的晶化阶段是不一样的,晶化初期为扩散控制的三维形核和晶粒生长的整体晶化,晶化中后期为一维形核和晶粒生长的表面晶化,形核率近似为零。研究了Fe63.5Co10Si13.5B9Cu1Nb3纳米晶粉芯的磁性与球磨时间之间的关系,结果表明:纳米晶粉芯的有效磁导率表现出较好的频率稳定性,而且随着球磨时间的增加而减小,品质因子在低频范围内随着频率的增加而增加,在约80 kHz达到峰值,然后随着频率的进一步增加而逐渐减小。     

Kinetic Aspects of the Nanocrystallization and Evolution of Microhardness in Al92-XNi8LaX Amorphous Alloys

Marginal glass forming Al-based alloys have attracted considerable attention due to the occurrence of a primary crystallization reaction that yields a microstructure consisting of uniformly dispersed Al-nanocrystals embedded in an amorphous matrix. Rapidly solidified Al-alloys ribbons containing 8 at.% Ni and 4-6 at.% La were prepared by single roller melt-spinning technique. As-melt-spun and annealed ribbons were investigated by means of differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and hardness measurements. XRD studies revealed that ribbons are fully amorphous in the as-melt-spun state. DSC studies showed that crystallization proceeds in two or three stages that are sensitively influenced by La content. Crystallizations kinetics were analysed by Kissinger and Johnson-Mehl-Avrami approaches. Microhardness of all the ribbons was examined at different temperatures and correlated with the corresponding structural evolution.     

Magneto-inductive element

A novel sensitive magnetic head using a magnetoinductive (MI) effect in zero- or negative-magnetostrictive amorphous wires is described. The MI effect refers to the change of an inductance L for an external magnetic field in a ferromagnetic wire element magnetized with a wire AC current I_AC. A 5-mm-length MI element using a folded almost zero-magnetostrictive amorphous wire having a 120-μm diameter showed a sensitive rate of change of its inductance of more than 50% for an external low frequency field of about 10 Oe (800 A/m) applied in parallel with the element. The a-wire MI element works for a wire current having frequencies up to 1 MHz     

Fe基非晶和纳米晶合金的热膨胀

将非晶Ｆｅ７３．５Ｃｕ１Ｎｂ３Ｓｉ１３．５Ｂ９和Ｆｅ９１Ｚｒ７Ｂ２合金经退火制成纳米晶合金，测量了淬火态和退火态样品的热膨胀曲线，研究了退火温度对热膨胀的影响，结果表明，纳米晶粒的形成导致居里温度Ｔｃ以下的热膨胀系数急剧增加，而Ｔｃ以上的热膨胀系数几乎不随退火温度变化。     

The migration behavior of atomic clusters in early nanocrystalline process of soft magnetic Finemet alloy

The Finemet alloys are commonly used as cores in transformers and generators, stress and field sensors in technological application for their excellent soft magnetic characteristics. To clarify the nanocrystallization mechanism of Finemet especially about the atomic migration in early stage is very essential for developing their distinctive characteristics. In this study, we investigate the migration behavior of atoms in order to clarify the mechanism of the early-stage nanocrystallization in amorphous Finemet alloys. The Fe(73.5)Si(13.5)B9Nb3Cu1 amorphous ribbons were prepared by single-roller melt-spinning process in argon atmosphere, and then annealed at 350 degrees C-400 degrees C for 10 minutes in vacuum. The atom force microscope (AFM) and the coincidence Doppler broadening spectra (CDB) were used to characterize the migration behavior of different atoms in Fe(73.5)Si(13.5)B9Nb3Cu1 amorphous alloy during the early-stage nanocrystallization. The X-ray diffraction (XRD) patterns show that all annealed samples are in the amorphous state. But the AFM observation shows clearly that there are many small atomic clusters (nuclei) which distribute in the amorphous matrix of the annealed samples. With increasing annealing temperature, there is a significant increase in the amount of atomic clusters and a dramatic drop in the average size of clusters with very limited Cu contention in the samples, which reflect the structural evolution into more homogeneity. The CDB spectrum indicates that the peaks of positron annihilation spectrum are gradually reduced, which means the number of grain boundary and the defects in samples are gradually increased. It can be concluded that more defects are introduced by the formation of atomic clusters through atomic migration during the early-stage nanocrystallization in Fe(73.5)Si(13.5)B9Nb3Cu1 amorphous alloys.     

Large electrical resistivity and high saturation magnetization nanocrystalline Fe86B13Cu1 alloy prepared by hot isothermal pressing

The effects of hot isothermal pressing (HIP) on the microstructures and magnetic properties of nanocrystalline Fe₈₆B₁₃Cu₁ ribbons were studied. It is shown that the precipitation of Fe₃B phase is suppressed and the grain size of α-Fe phase decreases to 13.2 nm when amorphous Fe₈₆B₁₃Cu₁ ribbons are annealed by HIP under the pressure of 150 MPa. A high electrical resistivity and high saturation magnetization nanocrystalline soft magnetic material is prepared by HIP owing to the suppression of the precipitation of Fe₃B phase and a marked decrease in the grain size of α-Fe phase. The prepared sample exhibits a large electrical resistivity of 183 μΩ cm, a high saturation magnetization of 1.94 T and a low coercive force of 12 A/m.     

Photoacoustic properties of softmagnetic amorphous Fe81B13Si4C2 ribbon

Photoacoustic properties of amorphous Fe81B13Si4C2 ribbons were investigated. The amplitude and phase photoacoustic spectra were measured as a function of the modulation frequency of an He–Ne laser beam. Thermal diffusivity was determined by comparison of obtained experimental results and calculated theoretical photoacoustic spectra for a non-annealed Fe81B13Si4C2 sample and an Fe81B13Si4C2 sample annealed at 600 °C. © 1998 Chapman & Hall