Magnetostatic properties of heterogeneous Co-based amorphous/crystalline phases

Using the magneto-optical Kerr effect, magnetic hysteresis loops are measured on annealed amorphous Co₆₆Fe₄B₁₅Si₁₅ samples, to characterize the magnetostatic properties of the heterogeneous crystalline/amorphous phases. A gradual change, on microscale inhomogeneous, change of the magnetic properties with respect to thickness is revealed on HCP-Co, FCC-Co crystalline phases near the surface. The inner amorphous phase exhibits an irregular variation of the local magnetic properties, presumably due to the occurrence and distribution of microcrystallites. The effective field, exerted by the crystalline layer on the amorphous phase, is opposite to the surface magnetization, indicating that there is an antiferromagnetic coupling between surface and inner amorphous phases.     

Crystallisation kinetics of amorphous Si–C–N ceramics: Dependence on nitrogen partial pressure

The crystallisation kinetics of amorphous precursor-derived ceramics of composition Si₂₆C₄₁N₃₃ is investigated as a function of temperature and nitrogen partial pressure using X-ray diffractometry. Isothermal annealing at a pressure of 1 bar leads to simultaneous crystallisation of Si₃N₄ and SiC, while only crystalline SiC is formed with annealing at a reduced pressure of 1 mbar. Rate constants of crystallisation are determined using the Johnson–Mehl–Avrami–Kolmogorov (JMAK) formalism. For temperatures below 1700°C, crystallisation rates are significantly higher for annealing at 1 mbar compared to 1 bar. For an explanation of the results, a model is proposed, which is based on diffusion-controlled nucleation and growth of crystalline Si₃N₄ and SiC in an amorphous matrix combined with thermal decomposition of Si₃N₄ at high temperatures.     

Crystallization of some amorphous metallic alloys studied by Mössbauer spectroscopy

The present work provides an analysis of crystallization processes in amorphous metallic alloys Fe₈₀Si₄Cr_1.0B₁₄ and Fe₆₇Co₁₈B₁₄Si₁. Crystallization of the first sample started at the temperature of 648 K. The fully crystalline state was observed after annealing at 748 K. We identified four sextets. One corresponds to crystalline Fe₂B and the three others to FeSi solid solution with 10 at .% of Si. Crystallization of Fe₆₇Co₁₈B₁₄Si₁ started at the temperature of 623 K. We identified two crystalline phases. The first may have its origin as (Fe_1−xCo_x)₃B, the second one may correspond to a Fe−Co solid solution with a different Co content.     

Stability of nanovoids in amorphous Si3B3N7

The amorphous ceramic material a-Si₃B₃N₇ possesses a rather low density (≈1.9?g/cm³) compared with, for example, the weighted average of the crystalline binary compounds Si₃N₄ and BN (≈2.8?g/cm³). Our simulations show that nanosize cavities, which are created during synthesis via the sol–gel route, can survive for a very long time even at elevated temperatures (up to 1500?K), and are thus the most likely explanation for the low density of a-Si₃B₃N₇. Furthermore, we find that, at low temperatures, the application of very high pressures exceeding 10?GPa should lead to a considerable irreversible densification of the material up to ≈2.8?g/cm³.     

Mössbauer study of isothermally annealed amorphous Fe-Nb-Cu-Si-B alloys

Amorphous ribbons of Fe_73.5Nb₃Cu₁Si_13.5B₉ have been annealed above the crystallization temperature. Annealed samples consisted of crystalline and amorphous phases in a wide temperature range. Two samples of different thicknesses of 33 µm and 27 µm were isothermally annealed at a temperature of 545°C from 0.5 to 5 h in a vacuum furnace. The amount of crystalline phase increases rapidly in the ticker sample. The crystalline part of the Mössbauer spectrum consists of four sharp sextets which can be assigned to a DO₃-structure FeSi alloy. After 700°C annealing the amorphous phase was not observed and the crystalline phase consisted of the DO₃-structure FeSi alloy, paramagnetic FeNbB and presumably Fe₂₃B₆ and Fe₃SiB₂.     

AlN/Si3N4纳米多层膜的外延生长与力学性能

采用射频磁控溅射方法制备单层AlN, Si₃N₄薄膜和不同调制周期的AlN/Si₃N₄纳米多层膜.采用X射线衍射仪、高分辨透射电子显微镜和纳米压痕仪对薄膜进行表征.结果发现,多层膜中Si₃N₄层的晶体结构和多层膜的硬度依赖于Si₃N₄层的厚度.当AlN层厚度为4.0nm、 Si₃N₄层厚度 关键词： 3N₄纳米多层膜')" href="#">AlN/Si₃N₄纳米多层膜 外延生长 应力场 超硬效应     

激光辐照非晶Fe73.5Cu1Nb3Si13.5B 9微量晶化的穆斯堡尔谱研究

在激光功率为40—160W、扫描速度为10mm/s、激光光斑为20mm照射条件下,用CO ₂激 光辐照非晶Fe_73.5Cu₁Nb₃Si_13.5B_{9< /sub>产生微量晶化.利用透射穆斯堡尔谱 （TMS）技术分析了原始态和晶化后样品的超精细结构.确定了穆斯堡尔谱的基本参数——化 学位移(IS)、四极分裂(QS)、内磁场(Hhf)随激光功率变化的规律.分析表明，CO2关键词： 激光辐照 微量晶化 73.5Cu1Nb3 Si13.5B9')" href="#">非晶Fe73.5Cu1Nb3 Si13.5B9 穆斯堡尔谱}     

Radio-frequency induced effects in amorphous and nanocrystalline Fe73.5Cu1Nb3Si13.5B9

The rf collapse and sideband effects are used to study the microstructure of the Fe_73.5Cu₁Nb₃Si_13.5B₉ alloy in the amorphous and nanocrystalline state. Nanocrystalline grains of -Fe(Si) are formed as a result of annealing of the amorphous alloy at 520–570 °C. The results show that the complete rf collapse of magnetic hfs in the Mössbauer spectra occurs only in the amorphous phase. The rf collapse is strongly affected by the onset of the nanocrystalline phase and is suppressed when the Fe₃B and Fe₂B phases are formed. Partial collapse allows us to follow the remaining crystalline fractions during the crystalline process. The rf sidebands disappear due to the formation of nanocrystals because of the vanishing magnetostriction.     

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     

Raman spectroscopic studies of LixSiy compounds

The phase diagram of the Li–Si system contains several phases with Li and Si in well defined ratios. So far, only the Raman spectrum of LiSi has been reported. In this work, we present experimental Raman scattering results for the crystalline lithium silicide phases Li₁₂Si₇, Li₇Si₃, Li₁₃Si₄, and Li₂₁Si₅/Li₂₂Si₅, which show clearly distinguishable Raman modes. The experimental results are compared with theoretical data obtained by density functional theory calculations. Copyright © 2013 John Wiley & Sons, Ltd.     

On the determination of the volume fraction of the crystalline phase in amorphous-crystalline alloys

The possibility of determining volume fractions of crystalline and amorphous phases of partially crystalline alloys from X-ray diffraction data has been discussed. The crystallization of an amorphous microwire of the Fe_73.9B_13.2Si_10.9C₂ composition has been investigated. The crystallization leads to the formation of α-Fe and Fe(Si). An analysis has been made of the X-ray diffraction patterns recorded for a series of samples with different contents of the crystalline and amorphous phases. The angular range has been determined and the calibration graph has been constructed, which can be used to determine the volume fractions of the amorphous and crystalline components in amorphous-crystalline samples.     

Structural and magnetic study of Mo-doped FINEMET

In this paper, a study of the structural and the magnetic correlation of the crystalline and amorphous phases in the nanocrystalline system Fe_73.5Si_13.5B₉Nb_3?xMo_xCu₁ (x=0, 1.5, 2, 3) was made. By means of Mössbauer spectroscopy, simple mass balance considerations and density measurements, both phases fractions and chemical compositions were calculated (in at%, wt% and vol%). Then, quasistatic magnetic measurements and ab initio calculations were used in a magnetic balance model in order to estimate the magnetic contribution of the remaining amorphous phase, which was compared to that of as-quenched amorphous samples of the same composition. The difference in both magnitudes showed the influence of penetrating fields and that these became more important for higher crystalline fractions.     

INVESTIGATION ON THE COMPOSITION AND STRUCTURE OF SILICON NITRIDE FILM PREPARED BY ECR-PECVD

In this paper, the effect of temperature on the composition and structure of the Si₃N₄ thin film is investigated. X-ray diffraction pattern and transmission electron microscope (TEM) analyses show that the Si₃N₄ film undergoes the transition from amorphous to crystalline phase with increasing deposition temperature. Infra-red qualitative analysis shows that the content of hydrogen decreases with increasing deposition temperature.The stoichiometric of Si₃N₄ is investigated by X-ray photoelectron spectroscopy or electron spectroscopy for chemical analysis.     

Intrinsic photoluminescence properties of amorphous Si3B3N7 ceramic

Amorphous Si₃B₃N₇ ceramic shows intrinsic photoluminescence. Three distinctive emission regions have been observed. Excitation with wavelengths between 254 and 330 nm stimulates intense blue emissions with peak maxima ranging from 447 to 479 nm. Exciting between 315 and 420 nm results in two broad emission peaks; the first in the range between 400 and 440 nm, and the second between 560 and 690 nm. Of these two latter emissions, the one in the violet region dominates in intensity over the other one in the red region, thus a violet color is perceived with the eye via excitation with 330 nm or higher wavelengths. The three distinct intrinsic emissions in the photoluminescence spectrum of amorphous Si₃B₃N₇ ceramic are related to defect centers in three topologically different regions in its structure. Dependence of emission on excitation wavelength is associated with the Red-Edge Effect and can be explained with a reabsorption mechanism at the red excitation edge.     

Nanosize silicon nitride: characteristic of doped powders and of the related sintered materials

The paper reports on both the characteristics of ultrafine silicon nitride powder produced by plasma synthesis and the microstructure and properties of the relative sintered material. The powder, already containing yttria and alumina as sintering aids, has a bimodal particle size distribution and it is partly amorphous. The chemical composition and morphology of the particles are shown. Yttria and alumina were not found in separate particles but the elements constituting them (i.e., Y, Al, O) are either in solid solutions in the crystalline particles or dispersed within the amorphous portion of the powder. Dense materials were obtained by pressureless sintering at 1750 °C. Microstructure and composition of silicon nitride grains and of grain boundary phases are analyzed and discussed. When compared to a micro-sized Si₃N₄, nanoindentation tests clearly revealed the inverse Hall Petch relation. The nanosize Si₃N₄ shows a Young’s modulus which is almost independent on the peak load. PACS 81.05.J,M; 81.40; 81.05.Y; 81.05.J; 46.30.P     

Studies of structure and morphology of sputter-deposited stainless steel–nitrogen films

Stainless steel films doped with nitrogen were deposited on heated and unheated (100) silicon substrates by radio-frequency magnetron sputtering of an austenitic stainless steel target in argon and nitrogen gas mixtures, containing a range of nitrogen compositions. The evolution of phases, morphologies and grain structures in the resultant films was studied by X-ray diffraction and field emission scanning electron microscopy. It was found that, with increasing nitrogen composition in the gas mixture, the crystalline structure of the films deposited on the heated substrates changed from bcc ferrite (α), to nitrogen-stabilized fcc austenite (γ), then to distorted expanded austenite phase (γ_N) with nitrogen supersaturation, and finally to the newly discovered fcc ‘MN’ phase with ideal cubic symmetry and further enlarged lattice. On the unheated substrates, the phase-evolution trend was found to be different for % N₂ above 10. For the 25% N₂ film, amorphous phase formed along with the crystalline austenite and ferrite phases, while the percentage of amorphous content decreased when % N₂ was increased to 50. This different trend was understood to be due to the role of increase in % N₂ in decreasing the energy loss of sputtered species through collisions. The dependence of crystalline phase formation on the energy of sputtered species is less severe on the heated substrates. Although all the films deposited experienced three-dimensional fibrous growths, they exhibited different surface morphology and grain structure. There exists a correlation between film morphology and phase constituents, while grain size was influenced by the nucleation density and the energy and mobility of adatoms that are reduced due to nitrogen incorporation. PACS 68.55.-a; 81.15.Cd     

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.     

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.