High-resolution FIB-TEM-STEM structural characterization of grain boundaries in the high dielectric constant perovskite CaCu3Ti4O12

In this work, the grain boundaries composition of the polycrystalline CaCu₃Ti₄O₁₂ (CCTO) was investigated. A Focused Ion Beam (FIB)/lift-out technique was used to prepare site-specific thin samples of the grain boundaries interface of CCTO ceramics. Scanning transmission electron microscopy (STEM) coupled with energy dispersive X-ray spectrometry (EDXS) and Electron Energy Loss Spectroscopy (EELS) systems were used to characterize the composition and nanostructure of the grain and grain boundaries region. It is known that during conventional sintering, discontinuous grain growth occurs and a Cu-rich phase appears at grain boundaries. This Cu-rich phase may affect the final dielectric properties of CCTO but its structure and chemical composition remained unknown. For the first time, this high-resolution FIB-TEM-STEM study of CCTO interfacial region highlights the composition of the phases segregated at grain boundaries namely CuO, Cu₂O and the metastable phase Cu₃TiO_4.     

Crack initiation and propagation in braided SiC/SiC composite tubes: Effect of braiding angle

Crack initiation and propagation in three braided SiC/SiC composite tubes with different braiding angles are investigated by in situ tensile tests with synchrotron micro-computed tomography. Crack networks are precisely detected after an image subtraction procedure based on Digital Volume Correlation. FFT based simulations are performed on the full-resolution 3D images to assess elastic stress/strain fields. Quantitative measurements of the crack geometries are performed using a novel method based on grey levels. The results show that braiding angle has no obvious effect on the location of crack onsets (initiation always occurs at tow interfaces), whereas it significantly affects the paths of crack propagation. This work provides an explicit demonstration of the crack propagation scenarios with respect to the mesoscopic fibre architectures.     

Deposition of boron-containing coatings by electron-beam evaporation of boron-containing targets

Boron-containing films are promising materials for improving the hardness, wear-resistance and durability of mechanical parts used in industry. We describe a novel approach for deposition of such coatings – by using electron-beam evaporation of boron-containing target material (pure boron or boron nitride) in inert (helium) or chemically-active (oxygen, nitrogen, residual atmosphere) gases at medium vacuum. Boron-containing films deposited on titanium substrates were characterized using a nanohardness tester and a non-contact 3D profilometer. Elemental composition of the coatings was studied using raster electron microscope equipped with a device for EDX analysis. All boron-containing coatings provided significant improvement (by a factor of 4–16) in the microhardness of the substrate surface.     

煤与高岭石表面性质对凝聚过程的影响机制

煤泥水中含大量高岭石等黏土矿物,为其絮凝沉降带来较大的困难。为明确矿物性质对凝聚过程的影响机制,在应用扩展的DLVO理论计算煤和高岭石颗粒间作用力的基础上,采用聚焦光束反射测量仪监测了CaCl2用量为4.50 mmol/L时20 g/L的煤和高岭石的悬浮液在60, 100和150 r/min的搅拌转速下的凝聚过程。结果表明,颗粒间的静电作用力在颗粒表面间距2?200 nm范围内起主导作用,高岭石的电负性较大,在凝聚过程中更难发生靠近和碰撞;较高的转速可为颗粒提供较大的动量,有利于提高碰撞频率,缩短完成凝聚所需时间,实验条件下,煤和高岭石的凝聚时间分别由74和123 s缩短至47和89 s。疏水性作用力在颗粒表面间距小于2 nm的范围内起主导作用,决定了颗粒的黏附效率;煤因强疏水性,在碰撞后更易黏附,且能抵抗更高的流体剪切作用,可由19.32 μm凝聚形成100 μm的大凝聚体,而高岭石则因其亲水性难以得到较大粒度的凝聚体,均小于30 μm。     

Preparation of bismuth nanowire encased in quartz template for Hall measurements using focused ion beam processing

ABSTRACT: Forming electrodes on opposite sides of an individual bismuth nanowire was attempted to prepare for Hall measurements. Although a 1-mm-long bismuth nanowire which is completely covered with a quartz template has been successfully fabricated to prevent oxidation, it is very difficult to attach Hall electrodes on the opposite sides of the nanowire due to the quartz covering. One side of the cylindrical quartz template was removed by polishing without exposure of the nanowire to the atmosphere; the thickness between the polished template surface and the nanowire was estimated to be several micrometers. Focused ion beam processing was successfully employed to expose both surfaces of the nanowire under high vacuum by removing part of the quartz template. A carbon thin film was then deposited in situ on the wire surface to fabricate an electrical contact on the bismuth nanowire sample. Furthermore, the energy dispersive X-ray analysis was performed to the area processed by focused ion beam, and the bismuth component of the nanowire was successfully detected. It was confirmed that the focused ion beam processing was applicable to attach electrodes to bismuth nanowire for Hall measurement.     

Investigation of properties of ZnO ceramics sintered from ZnO-Zn nanopowders produced by pulsed electron beam evaporation

In this paper we have studied the properties of ZnO ceramics sintered from the ZnO-Zn nanopowders (NPs) produced by a pulsed electron beam evaporation of heterogeneous targets (oxide or metal) and to establish the influence of NPs prehistory on the luminescence and dilatometry properties of ceramics produced from them. Pressing was performed on uniaxial presses: static and the magnetic pulsed one. Sintering of ceramics was produced in air by heating to 1200 °C in 60 min. Maximal density of the ceramics did not exceed 81,25% of the theoretical density. The behavior of the shrinkage curves of ZnO-Zn NPs depends on their prehistory. Evolution of properties of ZnO-Zn nanoparticles (NPles) during annealing in air is studied by XRD and pulsed cathodoluminescence methods. The suppression of the ultraviolet emission in NP obtained by electron beam evaporation, and in ceramics sintered of them was established.     

Generation and Evolution of Surface Oxide Layer of Amorphous Boron during Thermal Oxidation: A Micro/nanofabricated Slice Measurement

The generation and evolution of the surface oxide layer of boron were thoroughly investigated due to the key role of the oxide layer in ignition and combustion of amorphous boron (B). Samples in different oxidation degrees were obtained by heating B particles until 600, 650, and 700 °C, using a temperature programmed thermobalance. A dual beam focused ion beam micro/nanofabricator was used to etch and cut the samples into thin slices (ca. 327 nm). The slices were observed under a scanning transmission electron microscope, accompanied with energy dispersive X‐ray analysis. During the thermal oxidation process, B particles initially lost mass through dehydration. Then they began to get oxidized and gain weight markedly. The sample surface became more rough as the final temperature increased. Two different reaction modes took place in sequence during the thermal oxidation of the samples. Below 650 °C, the oxidation reaction occurred only on the surface of the particle (the surface reaction mode). However, when the samples were heated to 700 °C, the particle interior was also involved in the reaction (the global reaction mode), and a large number of pores were formed. The O content of the initial surface oxide layer was fairly high. The thickness distribution was uniform (average thickness 148.1 nm) and the two edges were both smooth. During the heating, the oxygen content of the surface oxide layer increased after an initial decrease. The average oxide layer thickness increased and the thickness distribution became irregular and unequal. The sample heated until 700 °C had an average surface oxide layer thickness of 379.3 nm, and the thickness span reached 354.3 nm. During the global reaction process (700 °C), the oxidation degree within the interior of the particle was lower than that on its surface. In the particle interior, pores near the center were smaller than those close to the edge, whereas the oxidation degree was uniformly distributed. Results in this work provide a deeper understanding of the surface oxide layer, which can potentially help improve the ignition and combustion features of B.     

Ferroelastic domain switching and R-curve behavior in lead zirconate titanate (Zr/Ti = 52/48)-based ferroelectric ceramics

In this work, ferroelastic domain switching and R-curve behavior in lead zirconate titanate (Nb/Ce co-doped Pb(Zr_0.52Ti_0.48)O₃, ab. PZT-NC)-based ferroelectric ceramics were investigated, using the indentation-strength-in-bending (ISB) method. Firstly, Vickers indentation test examined the notable fracture anisotropy of PZT-NC ceramics between the poling direction and its perpendicular direction, and the crack open displacement (COD) profiles in the two directions were also theoretically calculated from the indentation fracture mechanics. And then two kinds of ferroelastic domain switching modes (in-plane and out-of-plane) were used for explaining such anisotropic propagation behavior of indentation cracks. The subsequent three-point bending test illustrated the dependence of fracture strength on indentation load and the rising crack growth resistance curves (R-curves) in two directions. The resulted R-curves were fitted by the Hill's type Growth Function successfully, giving the reasonable values of crack extension exponential (n), plateau fracture toughness (K_max), and initial fracture toughness (K_ini). The in-plane ferroelastic domain switching was identified as a more significant toughening mechanism for PZT-NC ceramics than the out-of-plane switching due to more switchable domains.     

空腹箱形梁的整体稳定性分析

本文采用等效厚度的方法将加缀板的空腹箱形梁转换为闭口薄壁截面梁.按照乌曼斯基的理论,建立了闭口薄壁梁的侧扭屈曲总势能方程;从总势能驻值原理出发,导出了一个适用于各种荷载与各种支承条件的薄壁截面梁的临界弯矩表达式。     

根据拉伸性能预测铝合金板材的疲劳裂纹扩展速率

本文在郑修麟和Hirt提出的疲劳裂纹扩展公式基础上’结合铝合金疲劳裂纹扩展门槛值的经验公式,提出了一个根据拉伸性能预测铝合金板材疲劳裂纹扩展速率的新方法。大量实验数据与估算结果对比表明,本文提出的疲劳裂纹扩展速率估算式是可行、实用的。此外,本文还强调了疲劳裂纹扩展门槛值△K_(th)在疲劳寿命估算中的重要性和工程中的实用性。