Effects of the joining process on the microstructure and properties of liquid-phase-sintered SiC-SiC joints formed with Ti foil

The joining of liquid-phase sintered SiC (LPS-SiC) ceramics was conducted using spark plasma sintering (SPS), through solid state diffusion bonding, with Ti-metal foil as a joining interlayer. Samples were joined at 1400 °C, under applied pressures of either 10 or 30 MPa, and with different atmospheres (argon, Ar, vs. vacuum). It was demonstrated that the shear strength of the joints increased with an increase in the applied joining pressure. The joining atmosphere also affected on both the microstructure and shear strength of the SiC joints. The composition and microstructure of the interlayer were examined to understand the mechanism. As a result, a SiC-SiC joining with a good mechanical performance could be achieved under an Ar environment, which in turn could provide a cost-effective approach and greatly widen the applications of SiC ceramic components with complex shape.     

退火工艺对激光选区熔化成形Ti6Al4V合金组织及室温力学性能的影响

以Ti6Al4V球形粉末为原料,利用激光选区熔化成形方法制备了Ti6Al4V合金试样,采用光学显微镜、扫描电镜及力学性能测试等手段,研究了退火工艺对Ti6Al4V合金室温力学性能及组织的影响规律。结果表明: SLM成形沉积态Ti6Al4V合金室温抗拉强度超过1200 MPa,而平均断后伸长率仅为4.0%;在650 ℃下进行真空退火处理,合金的抗拉强度仍保持在1200 MPa左右,规定塑性延伸强度R_p0.2高于1150 MPa,但试样的断后伸长率<10%;而在750及800 ℃下进行真空退火处理,合金试样的抗拉强度降至1100 MPa左右,规定塑性延伸强度高于1050 MPa,伸长率达到甚至超过10%,材料的综合强韧性得到明显提升。随着真空退火加热温度和保温时间的增加,SLM成形Ti6Al4V合金原始β晶界逐渐变模糊,晶粒趋向于等轴化。与此同时,快速冷却转变的α′针状马氏体未出现明显地粗化。     

Origin of the temperature stability of dielectric constant in CaCu3Ti4O12

The temperature and dc bias stability of the dielectric constant and loss tangent of CaCu₃Ti₄O₁₂ samples sintered under different oxygen atmospheres are discussed. The results suggest that the metal-oxygen vacancy related defects not only provide the charge carriers for the conduction (defect doping) but also contribute to the huge permittivity in the way of defect dipoles repositioning under charge carrier hopping. The charge localization in a specific copper-oxygen vacancy defect complex is the reason of the huge and stable permittivity and low dielectric loss in the middle temperature range, 90 K-200 K (20 Hz), while the implementation of the large barrier layer height needs a contribution by the titanium oxygen vacancy related trap charges in the grain boundaries, which also lead to a second permittivity stable range in a higher temperature range 200 K–300 K.     

正电子湮没研究Al、Nb共掺CaCu3Ti4O12陶瓷高介电常数机理

关于CaCu₃Ti₄O₁₂陶瓷的高介电常数机理，目前广泛接受的是非本征的内阻挡层电容模型。该模型认为在多晶中元素变价、缺陷和非化学计量比等导致的半导化晶粒被绝缘晶界层，即内阻挡层所包围。其中内阻挡层的厚度对材料的介电性能影响较大，而扫描电子显微镜（SEM）测试表明样品晶界呈稀烂的果酱状，SEM难以测量晶界区域绝缘内阻挡层厚度。本文采用正电子湮没技术表征其厚度，通过对CaCu₃Ti₄O₁₂陶瓷共掺不同浓度的Al、Nb（CaCu₃Ti_4-xAl_0.5xNb_0.5xO₁₂，x=0.2%、0.5%、5.0%）改变其晶粒和晶界的微观结构，研究CaCu₃Ti₄O₁₂陶瓷高介电常数机理。正电子湮没结果显示，掺杂样品符合多普勒展宽谱S参数的变化趋势与平均寿命的变化趋势一致。x=0.5%掺杂样品的介电常数最高，其平均寿命、S参数和湮没长寿命成分均最小，阻挡层最薄。实验结果验证了描述CaCu₃Ti₄O₁₂陶瓷高介电常数机理的内阻挡层电容模型的预测。     

Stabilizing temperature-capacitance dependence of (Sr,Pb, Bi)TiO3-Bi4Ti3O12 solutions for energy storage

(1-x)Sr_0.7Pb_0.15Bi_0.1TiO₃-xBi₄Ti₃O₁₂ ((1-x)SPBT-xBIT, x = 0-0.125) bulk ceramics were developed and calcined via the solid-state method, aimed at the application of pulsed power capacitors. The phase structures, temperature stability, hysteresis loop, and discharge properties were systematically investigated. Considering both the temperature stability and dielectric properties, 0.925SPBT-0.075BIT bulk ceramics with a capacitance variation satisfying the X7R specification were developed for pulsed power capacitors. The energy storage density was 0.252 J/cm³, and the ceramics showed high temperature stability at 80 kV/cm. The discharge current waveforms of the 0.925SPBT-0.075BIT ceramics were recorded. A high discharge power density of approximately 1.01 × 10⁸ W/kg with an 8 Ω load resistor and short discharge period of 84 ns were achieved at 50 kV/cm. The good temperature stability properties and high power density show that the 0.925SPBT-0.075BIT ceramics are well suited for pulsed power capacitors with a wide temperature range.     

Dielectric,ferroelectric, and piezoelectric properties of lead-free Ba0.95Ca0.05Ti1-xZrxO3 ceramics

Abstract

Ba_0.95Ca_0.05Ti_1-xZr_xO₃ (BCTZO) ceramics were prepared by a solid state reaction method. The samples were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and X-ray absorption near edge structure (XANES). The ceramics exhibit a pure perovskite structure. The average grain size gradually decreases with increasing Zr concentration. XANES results indicate that the intensities of pre-edge peaks dropped with increasing Zr concentration. The BCTZO ceramic of x?=?0.05 has the optimum electrical properties with the maximum dielectric constant (ε'_m), remanent polarization (2P_r), coercive electric field (2E_c) and piezoelectric charge constant (d₃₃) of 7,244, 12.54 (μC/cm²), 5.29 (kV/cm) and 288 (pC/N), respectively.     

Enhanced electrochemical performance of LiNi0.8Co0.1Mn0.1O2 via titanium and boron co-doping

Titanium and boron are simultaneously introduced into LiNi_0.8Co_0.1Mn_0.1O₂ to improve the structural stability and electrochemical performance of the material. X-ray diffraction studies reveal that Ti⁴⁺ ion replaces Li⁺ ion and reduces the cation mixing; B³⁺ ion enters the tetrahedron of the transition metal layers and enlarges the distance of the [LiO₆] layers. The co-doped sample has spherical secondary particles with elongated and enlarged primary particles, in which Ti and B elements distribute uniformly. Electrochemical studies reveal the co-doped sample has improved rate performance (183.1 mAh·g^-1 at 1 C and 155.5 mAh·g^-1 at 10 C) and cycle stability (capacity retention of 94.7% after 100 cycles at 1 C). EIS and CV disclose that Ti and B co-doping reduces charge transfer impedance and suppresses phase change of LiNi_0.8Co_0.1Mn_0.1O_2.     

多级深度还原法制备Ti6Al4V合金粉体的基础研究

目前Ti6Al4V合金粉体的生产方法主要有雾化法、机械合金法和氢化脱氢法,它们都以Kroll法生产海绵钛为基础。使用钛的氧化物作为原料的熔盐电解法和金属热还原法仍处于研究阶段。本文依据变价金属Ti和V的氧化物在还原过程中逐级还原的特性,提出使用金属氧化物(TiO₂, V₂O₅)作为原料的多级深度还原法制备Ti6Al4V合金粉体的新思路。首先计算了TiO₂-V₂O₅-Mg-Ca体系的吉布斯自由能变,结果表明先进行镁热自蔓延反应,后进行钙热深度还原反应制备Ti6Al4V合金粉体在热力学上具备可行性。然后通过实验进行了的验证。镁热自蔓延反应产物酸浸后除去MgO可得到氧含量为15.84%的多孔Ti-Al-V-O前驱体。配入金属Ca后进行深度脱氧可得到低氧Ti6Al4V合金粉体(Al: 6.2wt.%, V: 3.64wt.%, O: 0.24wt.%, Mg: 0.01wt.%, Ca: < 0.01wt.%)。     

Mechanical high-energy treatment of TiNi powder and phase changes after electrochemical hydrogenation

The paper presents the results obtained for the effect of ball milling of Ti–Ni powder, which is close in composition to the equiatomic one, on electrochemical hydrogenation. It is shown that the average size of the powder particles measured by BET and laser diffraction methods is found to reduce during milling, while the average size of the powder particles measured by SEM changes to attain its minimum within 30-s milling due to destruction and subsequent aggregation of particles. The powder in its initial state consists of a mixture of TiNi (austenite, martensite), Ti₂Ni, and TiNi₃ phases, and after ball milling, an X-ray amorphous phase is formed. The CDD size of the TiNi phase (austenite) reduces from 25 to 4 nm. It is found that the lattice parameters of the TiNi (austenite) and Ni₃Ti phases do not change during electrochemical hydrogenation, whereas the crystal lattice parameter of the Ti₂Ni phase increases, which indicates the predominant interaction of hydrogen with the Ti₂Ni phase. The lattice parameter of the Ti₂Ni based phase corresponds to Ti₂NiH_0.5 and Ti₂NiH_0.8 hydrides depending on the milling time and hydrogenation time. It is found that there is an “incubation period” of hydrogenation of the Ti₂Ni phase, which attains 90 min.     

The dehydrogenation kinetics and reversibility improvements of Mg(BH4)2 doped with Ti nano-particles under mild conditions

Magnesium borohydride, Mg(BH₄)₂, is ball-milled with Ti nano-particles. Such catalyzed Mg(BH₄)₂ releases more hydrogen than pristine Mg(BH₄)₂ does during isothermal dehydrogenation at 270, 280, and 290 °C. The catalyzed Mg(BH₄)₂ also exhibits better dehydrogenation kinetics than the pristine Mg(BH₄)₂. Based on kinetics model fitting, the activation energy (E_a) of the catalyzed Mg(BH₄)₂ is calculated to be lower than pristine Mg(BH₄)₂. During partial dehydrogenation, the catalyzed Mg(BH₄)₂ releases 4.23 wt % (wt%) H₂ for the second dehydrogenation at 270 °C, comparing to 4.05, and 3.75 wt% H₂ at 280, and 290 °C. The reversibility of 4.23 wt% capacity is also one of the highest for Mg(BH₄)₂ dehydrogenation under mild conditions such as 270 °C as reported. 4 cycles of Mg(BH₄)₂ dehydrogenation are conducted at 270 °C. The capacities degrade during 4 cycles and tend to be stable at about 3.0 wt% for the last two cycles. By analyzing the hydrogen de/absorption products of the catalyzed sample, Mg(BH₄)₂ is found to be regenerated after rehydrogenation according to Fourier Transform Infrared (FTIR) spectroscopy. Ti nano-particles can react with Mg(BH₄)₂ during ball-milling and de/rehydrogenation. The products include TiH_1.924, TiB, and TiB₂, which can improve the dehydrogenation properties of Mg(BH₄)₂ from a multiple aspect.