Pyroelectric properties of BST/PLT composite thick films with addition of xPbO–(1 − x)B2O3 glass

The Ba_xSr_1−xTiO₃ (BST)/Pb_1−xLa_xTiO₃ (PLT) composite thick films (20 μm) with 12 mol% amount of xPbO–(1 − x)B₂O₃ glass additives (x = 0.2, 0.35, 0.5, 0.65 and 0.8) have been prepared by screen-printing the paste onto the alumina substrates with silver bottom electrode. X-ray diffraction (XRD), scanning electron microscope (SEM) and an impedance analyzer and an electrometer were used to analyze the phase structures, morphologies and dielectric and pyroelectric properties of the composite thick films, respectively. The wetting and infiltration of the liquid phase on the particles results in the densification of the composite thick films sintered at 750 °C. Nice porous structure formed in the composite thick films with xPbO–(1 − x)B₂O₃ glass as the PbO content (x) is 0.5 ≥ x ≥ 0.35, while dense structure formed in these thick films as the PbO content (x) is 0.8 ≥ x ≥ 0.65. The volatilization of the PbO in PLT and the interdiffusion between the PLT and the glass lead to the reduction of the c-axis of the PLT phase. The operating temperature range of our composite thick films is 0–200 °C. At room temperature (20 °C), the BST/PLT composite thick films with 0.35PbO–0.65B₂O₃ glass additives provided low heat capacity and good pyroelectric figure-of-merit because of their porous structure. The pyroelectric coefficient and figure-of-merit F_D are 364 μC/(m² K) and 14.3 μPa^−1/2, respectively. These good pyroelectric properties as well as being able to produce low-cost devices make this kind of thick films a promising candidate for high-performance pyroelectric applications.     

Design, fabrication and optical characterization of cerium oxide-magnesium fluoride double layer antireflection coatings on monocrystalline silicon substrates

Theoretical and experimental studies of a double layer antireflection coating deposited onto silicon wafers have been carried out. Magnesium oxide and cerium oxide fabricated by physical vapor deposition method have been applied as low- and high-refractive index materials. MgF₂–CeO₂–Si structures exhibited the reflectivity below 3% in the wavelength window from 0.5 μm to 1.2 μm. Theoretical simulations of spectral characteristics of the reflectivity of these coatings have been performed. A good correlation between experimental data and theoretical curves has been observed with the assumption that a thin SiO₂ layer of a thickness of 16 nm is formed onto Si substrates.     

Solid–liquid interdiffusion bonding between In-coated silver thick films

Solid–liquid interdiffusion (SLID) bonding between two pieces of In-coated silver thick films was investigated. The silver thick film was prepared by screen-printing of silver paste on an aluminum oxide substrate. Indium was coated in thickness ranging from 3 to 12 μm onto the silver thick films using thermal deposition (in vacuum). Two pieces of the In-coated thick films were placed in intimate contact (with a compressive stress of 0.04 MPa) and heated (at 180–250 °C) for various durations (600–3600 s) to undergo SLID bonding. Measurement of the bonding strength indicated that the SLID bond in 3-μm-In-coated thick-film couples is stronger than that in 8-μm-In-coated couples. X-Ray diffraction, scanning electron microscopy and electron probe microanalysis were used to analyze the bond. The stronger bond comprises a central zone of γ-Ag₂In sandwiched by two Ag films; the weaker bond comprises a central zone of AgIn₂ sandwiched by two layers of γ-Ag₂In. In the latter case, diffusion of excess indium from the coat into the interface between the silver film and alumina substrates is responsible for bond weakening. The development of microstructures in the SLID process for both strong and weak bonds is proposed.     

含Zn、Mg生物玻璃的制备及性能研究

采用溶胶-凝胶法,在58S生物玻璃的基础上,分别用0.5wt％的氧化镁和氧化锌取代氧化钙制备了含镁和含锌的生物玻璃.压制的试样分别在600、700和800℃煅烧以做强度测试,并分析了600和800℃煅烧后的物相组成.结果表明,三种试样煅烧至800℃仍为玻璃态,而镁锌的掺入大幅度提高了生物玻璃的强度,这主要是因为Mg-O和Zn-O具有比Ca-O高的键能.模拟体液浸泡试验表明,镁和锌降低了羟基磷灰石的早期成核速度,但并不影响其后期的生长.浸泡三天后所有样品表面都被羟基磷灰石覆盖,表明了样品具有良好的生物活性.     

固体氧化物燃料电池阳极的相转化流延制备和电化学性能研究

采用相转化流延一步制备了NiO-Zr_0.84Y_0.16O_2-δ (YSZ)阳极支撑层和功能层, 前者厚度为~700 μm, 含有沿厚度方向定向排列的开放直孔, 后者厚度为~60 μm。采用浆料涂膜法和高温共烧在阳极上制备厚度为15 μm的YSZ电解质薄膜, 丝网印刷制备YSZ-La_0.84Sr_0.16MnO_3-δ (LSM)(质量比50:50)阴极。所制备的单电池显示出较高的电输出性能。以H₂-3%H₂O为燃料和环境空气为氧化剂, 800 ℃时电池的峰功率密度达到891 mW/cm², 电池即使在高电流密度测试条件下也未出现明显的浓差极化, 这是由于其阳极具有开放直孔结构, 气相输运阻力小。     

Residual stress development in Pb(Zr,Ti)O3/ZrO2/SiO2 stacks for piezoelectric microactuators

The residual stress of multilayers in piezoelectric microelectromechanical systems structures influences their electromechanical properties and performance. This paper describes the development of residual stress in 1.6 μm Pb(Zr_0.52,Ti_0.48)O₃ (PZT)/0.3 μm ZrO₂/0.5 μm SiO₂ stacks for microactuator applications. The residual stresses were characterized by wafer curvature or load-deflection measurements. PZT and zirconia films were deposited on 4-in. (100) silicon wafers with 0.5 μm thick thermally grown SiO₂ by sol–gel processes. After the final film deposition, the obtained residual stress of PZT, ZrO₂, and SiO₂ were 100–150, 230–270, and − 147 MPa, respectively. The average stress in the stack was  80 MPa. These residual stresses are explained in terms of the thermal expansion mismatch between the layers and the substrate. Load-deflection measurements were conducted to evaluate localized residual stresses using released circular diaphragms. The load-deflection results were consistent with the average stress value from the wafer curvature measurements. It was found that more reasonable estimates of the stack stresses could be obtained when mid-point vertical deflection data below 6 μm were used, for diaphragms 0.8–1.375 mm in diameter.     

Optimum thickness of carbon stripper foils in tandem accelerator in view of transmission and lifetime

Optimum thickness of charge stripper foils installed at the terminal of a tandem accelerator has been investigated from the view of (1) charge stripping effect, (2) transmission of ions through accelerator, (3) lifetime of foils for the irradiation of ions. For this purpose, measurements have been done for (a) transmission of H, Li, O, Br and Au ions, passing through 12 UD Pelletron tandem accelerator for carbon stripper foils of 1.8–19.5 μg/cm² thickness, at terminal voltages of 5 and 10 MV, and (b) lifetime of 2–15 μg/cm² thick Tanashi foils developed by Sugai by irradiating Au ions at the terminal voltage of 10 MV. The results obtained are as follows: (a) From the view of above items (1) and (2), the optimum thickness of foils is 10 μg/cm² for ions of Z=1, several μg/cm² for Z=8, and less than a few μg/cm² for heavier ions. (b) From the view of item (3), the lifetime of Tanashi foils by means of new arc-discharge method is demonstrated to be much longer than that of commercial foils for foils thicker than about 5 μg/cm² thick. This superiority rapidly decreases with decreasing foil thickness, and at around 2 μg/cm², the lifetime of Tanashi foils is at the most 2.4 times longer than that of commercial foils.     

表面多孔Ti-羟基磷灰石/Ti-Ag生物梯度复合材料的制备与性能

采用放电等离子烧结技术制备表面多孔Ti-羟基磷灰石（HA）/Ti-Ag生物梯度复合材料,研究了不同HA含量对复合材料微观结构、界面结合、表面孔隙特征、力学性能及体外生物活性的影响及机制。结果表明,表面多孔Ti-HA/Ti-Ag复合材料中间基体合金主要由α-Ti和Ti₂Ag相组成,表面多孔层主要由α-Ti和HA相组成,同时还存在少量CaO、CaTiO₃、Ti₅P₃等反应相;表面多孔Ti-HA/Ti-Ag复合材料中间基体与表面多孔层形成稳定的冶金结合,但随着HA含量增加,反应相增多,界面结合变差,表面孔隙率和平均孔径呈增大趋势,导致平均抗压强度减小且弹性模量降低,因此过高的HA含量会导致材料力学性能下降;体外生物活性实验表明,表面多孔Ti-HA/Ti-Ag复合材料在人工模拟体液中浸泡7天后表面生成大量类骨磷灰石层,并且随着HA含量的增大,磷灰石形成能力明显增强。      

Ion formation by high velocity impacts on porous metal targets

In impact ionization studies the target normally consists of a metal surface of compact solid density. In the present experiments, we investigate the use of a layer of a highly porous structure of nanometre-sized grains, sometimes also called “metal black”, as an alternative target. In our comparative experiments, spherical iron particles (0.1<d_p<1.5 μm) were shot with velocities 2–30 km/s onto both a compact solid silver plate and a silver metal black layer of about 7 μm thickness (grain size 20–40 nm, mean density ≈1 g/cm³), deposited on a compact solid gold plate. Impact generated ions were analysed by means of time-of-flight mass spectrometry. The results reveal important advantages of the porous black layer, such as better mass resolution and a larger amount of ions from the impacting particle. Therefore metal blacks may be very suitable targets for the purposes of identification and characterisation of the impacting particle's composition. An attempt is made to give a physical explanation of the results in the frame of existing empirical ionization models. The study is part of a programme to improve devices for in-situ analysis of fast moving cosmic dust particles.     

四步法制备高质量硅基砷化镓薄膜

为了提高在硅基上外延砷化镓薄膜的质量和实验的可重复性, 我们提出了一种叫做四步生长法的新方法, 该方法是通过在低温成核层和高温外延层中间先后插入低温缓冲层和高温缓冲层实现的。通过此方法, 可以制备出表面具有单畴结构、在强白光下依然光亮如镜、粗糙度低且缺陷少的高质量砷化镓薄膜, 而且此方法的重复性很好。即便没有任何生长后的退火处理, 外延出的1 μm厚砷化镓薄膜在5 μm×5 μm扫描区域内的表面粗糙度只有2.1 nm, 且由X射线双晶衍射测试出的砷化镓(004)峰的半高宽只有210.6 arcsec。     

Effect of microarc oxidised layer thickness on plain fatigue and fretting fatigue behaviour of Al–Mg–Si alloy

The objective of this work was to investigate the performance of microarc oxide coatings of two different thicknesses (40 and 100 μm) on Al–Mg–Si alloy samples under plain fatigue and fretting fatigue loadings. Tensile residual stress present in the substrate of 40 μm thick coated samples induced early crack initiation in the substrate and so their plain fatigue lives were shorter than those of untreated specimens. Presence of more pores and tensile surface residual stress in 100 μm thick coated samples caused early crack initiation at the surface leading to their inferior plain fatigue lives compared with 40 μm thick coated samples. While the differences between the lives of coated and uncoated specimens were significant under plain fatigue loading, this was not the case under fretting fatigue loading. This may be attributed to relatively higher surface hardness of coated specimens. The performance of 40 μm thick coated samples was better than that of 100 μm thick coated specimens under both plain fatigue and fretting fatigue loadings.     

Properties of piezoelectric actuator on silicon membrane, prepared by screen printing method

Characteristics of piezoelectric actuator on Si membrane were investigated. Si membranes were fabricated as a function of size using bulk micromachining method. Bottom electrode Ag–Pd and piezoelectric thick films were fabricated using screen printing method, respectively. Piezoelectric thick films were sintered by rapid thermal annealing (RTA). Top electrodes Pt were deposited by DC sputtering system. We analyzed micro structure by scanning electron microscope (SEM) and investigated dynamic properties by MTI2000. Therefore, piezoelectric thick film on Si membrane had P_r of 15.7 μC cm⁻². The maximum displacement of micro actuator had 0.05 μm. We find the combination of thick film printing and MEMS process to form a Si membrane micro actuator.     

Ba(Zr0.15Ti0.85)O3厚膜的介电与铁电性能研究

本研究采用流延法制备Ba(Zr_0.15Ti_0.85)O₃(BZT)厚膜样品。采用扫描电子显微镜分析样品形貌; 采用LCR测试仪和Sawyer-Tower电路法测量样品的介电与铁电性能。结果表明, BZT厚膜具有明显的介电弛豫特征, 击穿电场强度可达60 kV/cm以上, 饱和极化强度可达58.1 μC/ cm², 剩余极化强度(Pr)为20.9 μC/ cm²。     

Microstructures, densification and mechanical properties of TiC–Al2O3–Al composite by field-activated combustion synthesis

Dense TiC–Al₂O₃–Al composite was prepared with Al, C and TiO₂ powders by means of electric field-activated combustion synthesis and infiltration of the molten metal (here Al) into the synthesized TiC–Al₂O₃ ceramic. An external electric field can effectively improve the adiabatic combustion temperature of the reactive system and overcome the thermodynamic limitation of reaction with x < 10 mol. Thereby, it can induce a self-sustaining combustion synthesis process. During the formation of Al₂O₃–TiC–Al composite, Al is molten first, and reacted with TiO₂ to form Al₂O₃, followed by the formation of TiC through the reaction between the displaced Ti and C. Highly dense TiC–Al₂O₃–Al with relative density of up to 92.5% was directly fabricated with the application of a 14 mol excess Al content and a 25 V cm⁻¹ field strength, in which TiC and Al₂O₃ particles possess fine-structured sizes of 0.2–1.0 μm, with uniform distribution in metal Al. The hardness, bending strength and fracture toughness of the synthesized TiC–Al₂O₃–Al composite are 56.5 GPa, 531 MPa and 10.96 MPa m^1/2, respectively.     

Fabrication of a depletion mode GaAs MOSFET using Al2O3 as a gate insulator through the selective wet oxidation of AlAs

A 1 μm thick undoped GaAs buffer layer, a 1500 Å thick n-type GaAs layer, an undoped 500 Å thick AlAs layer and a 50 Å thick GaAs cap layer were consecutively grown by molecular beam epitaxy (MBE) on a [100] oriented semi-insulating GaAs substrate. The AlAs layer was oxidized in a N₂ bubbled H₂O vapor ambient at 400°C for 3 h and fully converted to Al₂O₃ for use as a gate insulator. The I–V characteristics, having a maximum drain current of 10.6 mA, a current cut-off voltage of −4.5 V and a maximum transconductance value of 11.25 mS/mm, indicate that the selective wet thermal oxidation of AlAs/GaAs was successful in producing a depletion mode GaAs MOSFET.     

Intense visible photoluminescence from coloured LiF films on silicon

Lithium fluoride films, about 1.5 μm thick, thermally evaporated onto silicon <100> substrates were subjected to low energy electron bombardment. Intense photoluminescence, extending from green to red in the visible spectral range was measured at room temperature in the irradiated areas, due to the presence of the laser active F₂ and F₃⁺ colour centres.     

Enhanced ferroelectric properties of multilayer SrBi2Ta2O9/SrBi2Nb2O9 thin films for NVRAM applications

Ferroelectric SrBi₂Ta₂O₉/SrBi₂Nb₂O₉ (SBT/SBN) multilayer thin films with various stacking periodicity were deposited on Pt/TiO₂/SiO₂/Si substrate by pulsed laser deposition technique. The X-ray diffraction patterns indicated that the perovskite phase was fully formed with polycrystalline structure in all the films. The Raman spectra showed the frequency of the O–Ta–O stretching mode for multilayer and single layer SrBi₂(Ta_0.5Nb_0.5)₂O₉ (SBNT) samples was 827–829 cm⁻¹, which was in between the stretching mode frequency in SBT (813 cm⁻¹) and SBN (834 cm⁻¹) thin films. The dielectric constant was increased from 300 (SBT) to 373 at 100 kHz in the double layer SBT/SBN sample with thickness of each layer being 200 nm. The remanent polarization (2P_r) for this film was obtained 41.7 μC/cm², which is much higher, compared to pure SBT film (19.2 μC/cm²). The coercive field of this double layer film (67 kV/cm) was found to be lower than SBN film (98 kV/cm).     

In vitro apatite formation on polyamide containing carboxyl groups modified with silanol groups

Modification of organic polymer with silanol groups in combination with calcium salts enables the polymer to show bioactivity, that is, the polymer forms apatite on its surface after exposure to body environment. However, how modification with silanol groups influences ability of apatite formation on the polymer substrate and adhesive strength between polymer and apatite is not yet known. In the present study, polyamide containing carboxyl groups was modified with different amounts of silanol groups, and its apatite-forming ability in 1.5SBF, which contained ion concentrations 1.5 times those of simulated body fluid (SBF), was examined. The rate of apatite formation increased with increasing content of silanol groups in the polyamide films. This may be attributed to enhancement of dipole interactions. A tendency for the adhesive strength of the apatite layer on the polyamide film to be decreased with increasing content of silanol groups was observed. This may be attributed to swelling in 1.5SBF and having a high degree of shrinkage after drying. These findings clearly show that modification of organic polymers with the functional groups induces apatite deposition, and also determines the adhesive strength of the apatite layer to the organic substrates.     

Bioresorbable and bioactive composite materials based on polylactide foams filled with and coated by Bioglass® particles for tissue engineering applications

Poly(DL-lactide) (PDLLA) foams and bioactive glass (Bioglass®) particles were used to form bioresorbable and bioactive composite scaffolds for applications in bone tissue engineering. A thermally induced phase separation process was applied to prepare highly porous PDLLA foams filled with 10 wt % Bioglass® particles. Stable and homogeneous layers of Bioglass® particles on the surface of the PDLLA/Bioglass® composite foams as well as infiltration of Bioglass® particles throughout the porous network were achieved using a slurry-dipping technique. The quality of the bioactive glass coatings was reproducible in terms of thickness and microstructure. In vitro studies in simulated body fluid (SBF) were performed to study the formation of hydroxyapatite (HA) on the surface of the PDLLA/Bioglass® composites, as an indication of the bioactivity of the materials. Formation of the HA layer after immersion in SBF was confirmed by X-ray diffraction and Raman spectroscopy measurements. The rate of HA formation in Bioglass®-coated samples was higher than that observed in non-coated samples. SEM analysis showed that the HA layer thickness rapidly increased with increasing time in SBF in the Bioglass®-coated samples. The high bioactivity of the developed composites suggests that the materials are attractive for use as bioactive, resorbable scaffolds in bone tissue engineering.     

Growth and structure in abalone shell

The growth and self-assembly of aragonitic calcium carbonate found in the shell of abalone (Haliotis) is described. This was accomplished through the close examination of laboratory-grown flat pearl samples and cross-sectional slices of the nacreous shell. Further understanding of the sequenced assembly has been obtained. It has been confirmed that the growth of the aragonite component of the composite occurs by the successive nucleation of aragonite crystals and their arrest by means of a protein-mediated mechanism; it takes place in the “Christmas-tree pattern” [Nature 49 (1994) 371]. It is shown that the protein layer is virtually absent where plates on a same plane abut (along lateral surfaces of tiles). This suggests a mechanism of c-axis aragonite growth arrest by the deposition of a protein layer of approximately 20–30 nm that is periodically activated and determines the thickness of the aragonite platelets, which are remarkably constant (0.5 μm). This platelet size was measured for animals with shell diameters of 10, 50, and 200 mm and was found to be constant. The overall growth process is expressed in terms of parameters incorporating the anisotropy of growth velocity in aragonite (V_c, the velocity along c axis, and V_ab, the velocity in basal plane). Comparison of laboratory-raised and naturally-grown abalone indicates growth regulated by the level of proteinaceous saturation. Naturally-grown abalone exhibits mesolayers (growth bands) 0.3 mm apart; it is proposed that they result from seasonal interruptions in feeding patterns, creating thicker (10–20 μm) layers of protein. These mesolayers play a critical role in the mechanical properties, and are powerful crack deflectors. The viscoplastic deformation of the organic inter-tile layers is responsible for the significant improvement of tensile strength over the tensile strength of monolithic aragonite.