Effects of Sm substitution on ferroelectric domains and conductivity in bismuth ferrite ceramics

The large piezoelectric coefficient and multiferroicity of bismuth ferrite (BFO) make it an attractive candidate for lead-free ferroelectric devices. However, large leakage currents have limited broader applications. Rare-earth substitutions in BFO have been shown to improve ferroelectric and magnetic properties. In this work, we employed piezoresponse and conductive atomic force microscopy to study ferroelectric domains in Bi_1-xSm_xFeO₃ (x = 0–0.150) grown by the co-precipitation method. The combined piezoresponse and conductivity measurements can directly visualize the local ferroelectric domains under different sample bias. At Sm mol% > 7.5, Sm-substitution effectively lowers defect-generated conductivity. At Sm mol% < 7.5, conductivity increases due to conductive domain walls inside sample grains. The surfaces of these conductive samples exhibit a p-type rectifying behavior while the bulk is n-type. Our work details how the local piezoelectric properties and transport behaviors of BFO ceramics change as a function of Sm-substitution.     

Pressure-driven transient flows of Newtonian fluids through microtubes with slip boundary

Recent advances in microscale experiments and molecular simulations confirm that slip of fluid on solid surface occurs at small scale, and thus the traditional no-slip boundary condition in fluid mechanics cannot be applied to flow in micrometer and nanometer scale tubes and channels. On the other hand, there is an urgent need to understand fluid flow in micrometer scale due to the emergence of biochemical lab-on-the-chip system and micro-electromechanical system fabrication technologies. In this paper, we study the pressure driven transient flow of an incompressible Newtonian fluid in microtubes with a Navier slip boundary condition. An exact solution is derived and is shown to include some existing known results as special cases. Through analysis of the derived solution, it is found that the influences of boundary slip on the flow behaviour are qualitatively different for different types of pressure fields driving the flow. For pressure fields with a constant pressure gradient, the boundary slip does not alter the interior material deformation and stress field; while, for pressure fields with a wave form pressure gradient, the boundary slip causes the change of interior material deformation and consequently the velocity profile and stress field. We also derive asymptotic expressions for the exact solution through which a parameter is identified to dominate the behaviour of the flow driven by the wave form pressure gradient, and an explicit formulae for the critical slip parameter leading to the maximum transient flow rate is established.     

Distinct ferroelectric domain switching dynamics in epitaxial BiFeO3 (001) capacitors depending on the bias polarity

Understanding ferroelectric domain switching dynamics at the nanoscale is a great of importance in the viewpoints of fundamental physics and technological applications. Here, we investigated the intriguing polarity-dependent switching dynamics of ferroelectric domains in epitaxial BiFeO₃ (001) capacitors using transient switching current measurement and piezoresponse force microscopy. We observed the distinct behavior of nucleation and domain wall motion depending on the polarity of external electric bias. When applying the negative bias to the top electrode, the sideways domain wall motion initiated by only few nuclei was dominant to polarization switching. However, when applying the positive bias, most of domains started to grow from the pre-existed pinned domains and their growth velocity was much smaller. We suggest that the observed two distinct domain switching behavior is ascribed to the interfacial defect layer.     

Pulse-controlled generation and characterization of partially-switched multiple-value polarization states in PZT ceramics

This paper explores in depth the partially switched states of ferroelectrics, through macroscopic polarization measurements in conjunction with piezoresponse force microscopy, x-ray diffraction and dielectric characterization, with the ultimate purpose to explore their usefulness for unconventional multiple-value nonvolatile memory applications. We prove that it is possible to reproducibly generate analog levels of polarization in a Pb(Zr,Ti)O₃ ferroelectric ceramic capacitor and control them with electric pulses that stabilize unique domain patterns, compatible with those of adjacent states. Some of these states contain, in the same locations of the sample surface, areas with orientation of polarization vector opposite to that of the electric field that decides the analog polarization level, while others contain clamped domain structures with reduced piezoelectric activity. We argue that disclosing the complex relationships between the domain structures of the analog polarization states, as well as their dependence on write voltage parameters, might help to expand the multiple-value storage capability of ferroelectrics beyond what would be achievable on macroscopic scale.     

Synthesis and properties of aligned ZnO microtube arrays

Two kinds of different aligned zinc oxide (ZnO) crystal microtube arrays were prepared on silicon (1 0 0) substrates by using of a simple thermal chemical reaction vapor transport deposition method. The synthesizing processes were done by using of heating the mixture of zinc oxide and graphite powders at 1150 °C in a quartz tube with one side opened to the air. The O₂ gas (99.9%) and air had been introduced as the assistant gases, respectively. Both the flow rates were 100 ml/min. And the temperature of the Si (1 0 0) substrate region was about 400 °C. There is no other metal catalyst on the Si wafers in the process. After growing for 30 min, one kind of synthesized sample is trumpet-shaped hexagonal microtube arrays assisted with O₂ gas and another produced sample is the uniform hexagonal microtubes only assisted with air. As the increasing of preparing time, their maximal lengths can range from several 10 μm to mm scale. The microstructure, room temperature photoluminescence properties and growth mechanism of both aligned microtube arrays were investigated and discussed.     

The effect of annealing temperature on the morphology and piezoelectric characteristics of BaTiO3 nanofibers and domain switching under different temperatures

Effects of annealing temperature (600–750 °C) on crystalline structure, the morphology and piezoresponse hysteresis loops of BaTiO₃ nanofibers prepared by electrospinning are characterized by X-ray diffraction, scanning electronic microscopy, transmission electron microscope and piezoresponse force microscope. When the annealing temperature is 700 °C, the nanofibers become smoother and have a diameter of 100–300 nm. Meanwhile the typical butterfly-shaped amplitude loop and 180°phase change represents the best ferroelectric and piezoelectric properties at 700 °C. So the 700 °C was found to be optimum for good piezoelectric characteristics at annealing temperature of 600 °C–750 °C. In order to give more clear evolution of domain states at different external fields, the three dimensional topographic and phase images of the nanofiber at different temperatures are observed by piezoresponse force microscope. The 90° domain switching is observed during heating from room temperature to 125 °C and the domain switching tends to be stable when the temperature exceeds a critical value. The thermal stress due to the high temperatures is responsible for switching mechanism from the perspective of equilibrium state free energy. This work suggests that the temperature variation should be considered while designing the ferroelectric devices based on one dimensional material.     

TEM study on hollow and prepared from porous Cu20 nanoparticles solution phase

In this paper, hollow and porous Cu2O nanoparticles were prepared by adjusting the cationic surfactant cetyltrimethylammonium （CTAB） concentration in the solution-phase reaction. Structural investigations reveal that Cu2Onanoparticles can be either well-defined hollow nanoboxes or porous nanocubes depending on the synthesis conditions. The transmission electron microscopy （TEM） observations demonstrated that the nanoparticles in general are composed of small grains coherently growing along certain preferred orientations.     

Cobalt sorption properties of MgO prepared by solution combustion

Water effect on the combustion preparation of MgO is presented. The obtained materials are characterized through their specific surface area, morphology, particle shape, fractal dimension and Co²⁺ sorption. The surface fractal dimension of the combustion prepared sample was 2.0 but in those where water was included it decreased to 1.8. In the sample prepared by calcination it was 2.3. A linear correlation between the fractal dimension and Co²⁺ sorption was found.     

Experimental investigation on the structural,dielectric, ferroelectric and piezoelectric properties of La doped ZnO nanoparticles and their application in dye-sensitized solar cells

Pure and lanthanum (La) doped ZnO nanorods were synthesized via co-precipitation method. The structure and morphology of as grown ZnO and La-ZnO nanoparticles were studied using transmission electron microscopy (TEM) and powder X-ray diffraction (XRD) methods. The values of remnant polarization and coercive field were found to be 0.027 μC/cm² and 1.33 kV/cm, respectively, for as grown La-ZnO nanostructures. High Curie temperature (276 °C) for doped ZnO was observed in dielectric study. Piezoelectric coefficient at room temperature was found to be 101.30 pm/V. I-V characteristics were studied for both pure and doped ZnO nanoparticles. Photo-anodes of dye-sensitized solar cells (DSSCs) were made using ZnO and La-ZnO nanorods. The conversion efficiency and short circuit current density of La-ZnO nanorods based DSSC were 0.36% and 1.31 mA/cm², respectively, which were found to be largely enhanced when compared with that of pure ZnO based DSSC (0.20% and 0.94 mA/cm²).     

Microscopical investigations of nisin-loaded nanoliposomes prepared by Mozafari method and their bacterial targeting

Nanoencapsulation may improve activity of protein or polypeptide antimicrobials against a variety of microorganisms. In this study, nanoliposomes prepared from different lipids (Phospholipon 90H, Phospholipon 100H, dipalmitoylphosphatidylcholine (DPPC), stearylamine (SA), dicetyl phosphate (DCP) and cholesterol) by a new, non-toxic and scalable method, were tested for their capacity to encapsulate nisin Z and target bacteria (Bacillus subtilis and Pseudomonas aeruginosa). Factors affecting the entrapment efficiency (charge and cholesterol concentration in the vesicles) and stability of nanoliposomes were assessed. The nanoliposomes and their bacterial targeting were visualised, using different microscopes under air and liquid environments. Nisin was entrapped in different nanoliposomes with encapsulation efficiencies (EE) ranging from 12% to 54%. Anionic vesicles possessed the highest EE for nisin while increase in cholesterol content in lipid membranes up to 20% molar ratio resulted in a reduction in EE. Stability of nanoliposome-encapsulated nisin was demonstrated for at least 14 months at 4 °C (DPPC:DCP:CHOL vesicles) and for 12 months at 25 °C (DPPC:SA:CHOL vesicles).     

Magnetic properties of cobalt substituted M-type barium hexaferrite prepared by co-precipitation

The co-precipitation and solid state methods were used in the synthesis of barium hexaferrite (BaM). Phase pure BaM was obtained with 1, 2, 3, 5, 10, 15, 20 and 30 wt% cobalt oxide (Co₃O₄). The addition of Co^2+/3+ ions to the BaM increased the permeability and magnetic loss tangent to a value of 3.5 at 5% and reduced to 1 at 30% doping. With increased Co doping, M_s was reduced from 87-58 emu/g, M_r increased from 11 to 40 emu/g with 3–5 wt% Co and 9 emu/g for 30% doping. H_c sharply increased from 540 to 2200 Oe with a reduction to 280 Oe at 10 K with increasing temperature to 300 K. T_c increased from 740 to 750 K for 30% Co doping. DTA–TGA studies of green body showed decarboxilation to occur at around 825 °C and the transformation of residual Co₃O₄ to Co₂O₃ at around 577 °C. The XRD data confirmed the Co ions substituting into Fe sites until a 10–15% doping level where the structure altered to W-type hexaferrite. The densities of the compounds varied with doping to a maximum of 4.45 g/cm³.     

Superdomain structure and high conductivity at the vertices in the (111)-oriented epitaxial tetragonal Pb(Zr,Ti)O3 thin film

Recently, in ferroelectric materials, there have been many experimental efforts to find out more intriguing topological objects and their functionalities, such as conduction property. Here we investigated ferroelectric domain structures and related topological defects in the (111)-oriented epitaxial tetragonal PbZr_0.35Ti_0.65O₃ thin film. Systematic piezoresponse force microscopy measurements revealed that the field-induced polarization switching can form thermodynamically stable superdomain structures composed of nano-sized stripe subdomains. Within such superdomain structures, we observed the exotic equilateral triangular in-plane flux-closure domains composed of three stripe domain bundles with 120/120/120 degrees of separation. The conductive-atomic force microscopy measurements under vacuum showed that some vertices have significantly higher conductivity compared to other surrounding regions. This work highlights electric field-driven polarization switching and unique crystallographic symmetry (here, three-fold rotational symmetry) can generate exotic ferroelectric domain structures and functional topological defects, such as conductive vertices.     

机械剥离折叠石墨烯粘附与纳米摩擦性质

本文用原子力显微镜研究了空气和氮气两种不同气氛环境下的机械剥离石墨烯粘附力,发现氮气环境下的粘附力更小,且石墨烯边缘的粘附力比内部区域大.在氮气环境下探究了折叠石墨烯粘附力与层数的关系及其摩擦性能,结果表明粘附力与折叠石墨烯层数无明显关系,折叠石墨烯各区域的摩擦性能都远超二氧化硅基底,且单层、单层上折叠、双层以及双层上折叠区域的摩擦系数依次降低,分别为0.049,0.031,0.023和0.021,摩擦力也依次降低,折叠处由于层与层之间的结合力弱于相同层数的石墨烯,摩擦性能有所降低,但未发现粘附力与摩擦力之间的明显关系.在采用尖针和球针测量粘附力时,测量历史不会对后续粘附力产生明显影响.对空气环境下出现的新鲜折叠石墨烯的研究表明新鲜折叠石墨烯的折叠区域摩擦力较未折叠区域显著增大.     

自组装硫醇分子膜电输运特性的导电原子力显微镜研究

在Au(111)表面自组装制备了不同链长的烷烃硫醇分子膜，并利用导电原子力显微镜研究了 自组装分子膜的输运特性随外加压力的变化.结果发现分子膜的电流随压力的增加而增大， 其变化特征可以较好地用Hertz模型描述.在相同压力和电压下，通过分子膜的电流随分子链 长的增加呈指数衰减，其衰减因子先随压力的增加而减小，后逐渐趋于稳定.此外，长链分 子自组装膜的电流随压力的变化比短链分子膜更为明显.分析表明，自组装硫醇分子膜输运 特征的压力依赖性主要源于电荷在分子膜中的链间隧穿过程. 关键词： 分子自组装 输运特性 原子力显微镜     

Nanoporous alumina membrane prepared by nanoindentation and anodic oxidation

The fabrication of nanopatterned surfaces at large scale attracts the interest of research groups from a wide range of areas as biotechnology, nanoelectronics and nanomagnetism. An extended method to pattern the surface in the nanoscale is the fabrication of ordered arrays of nanoelements based on porous templates as Nanoporous Anodic Aluminium Oxide (NAAO). One of the challenges of the NAAO fabrication, based on self-organized methods, is the control of the symmetry and lattice parameter of the ordered nanoporous films. In this work, we present a combined method based on Atomic Force Microscopy (AFM) nanoimprint and anodic oxidation of Al surface. AFM nanoindentations substitute the first anodization process and even more important, allow us to control the symmetry and the lattice parameter of the ordered arrays. In addition, by using AFM nanoimprint method it is possible to select the region were the ordered alumina grows. We demonstrate that square nanoporous arrays of alumina with lattice parameter of 105 nm can be obtained by this method.     

Surface properties of diamond-like carbon films prepared by CVD and PVD methods

Diamond-like carbon (DLC) films have been deposited using three different techniques: (a) electron cyclotron resonance---plasma source ion implantation, (b) low-pressure dielectric barrier discharge, (c) filtered---pulsed cathodic arc discharge. The surface and mechanical properties of these films are compared using atomic force microscope-based tests. The experimental results show that hydrogenated DLC films are covered with soft surface layers enriched with hydrogen and sp$^{3}$ hybridized carbon while the soft surface layers of tetrahedral amorphous carbon (ta-C) films have graphite-like structure. The formation of soft surface layers can be associated with the surface diffusion and growth induced by the low-energy deposition process. For typical CVD methods, the atomic hydrogen in the plasmas can contribute to the formation of hydrogen and sp$^{3}$ hybridized carbon enriched surface layers. The high-energy ion implantation causes the rearrangement of atoms beneath the surface layer and leads to an increase in film density. The ta-C films can be deposited using the medium energy carbon ions in the highly-ionized plasma.     

Optical properties of GdTaO4:Eu thick films prepared from a PVP-containing solution

Transparent GdTaO₄:Eu³⁺ thick films were prepared from the inorganic salt and 2-methoxyethanol solution containing polyvinylpyrrolidone (PVP) via sol-gel technique. The critical thickness of the film, i.e. the maximum thickness achievable without crack formation via non-repetitive deposition, was 0.8 μm. The effect of PVP on the morphology, crystallization behavior and optical property of the GdTaO₄:Eu³⁺ thick film was investigated. The results indicated that PVP could play an important role in the formation of transparent GdTaO₄:Eu³⁺ thick films, suppressing the stress evolution, adjusting the sol viscosity, ameliorating the crystallinity, and strengthening the covalency of Eu-O bonds. The GdTaO₄:Eu³⁺ thick films prepared with PVP exhibited a superior photoluminescence and X-ray exited luminescence, which implies that it will have promising applications in high-spatial-resolution X-ray imaging and flat panel display devices.     

Exact second order formalism for the study of electro-acoustic properties in piezoelectric structures under an initial mechanical stress

In this study we develop the exact second order formalism of piezoelectric structures under an external mechanical stress. Indeed, previous models are approximated since they consist in deriving all the equations in the natural coordinate system (corresponding to the pre-stress free case). Hence, our exact formalism proposes to obtain the whole of equations in the current coordinate system (which is the coordinate system after the pre-deformation). Then, this exact formalism is used to derive the modified Christoffel equations and the modified KLM model. Finally, we quantify the correction with the approximate formalism on several transfer functions and electro-mechanical parameters for a non hysteretic material (lithium niobate). In conclusion, we show that for this material, significant corrections are obtained when studying the plane wave velocities and the electrical input impedance (about 4%), whereas other parameters such as coupling coefficient and impulse response are less influenced by the choice of coordinate systems (corrections less than 0.5%).     

Annealing effects on microstructural and optical properties of Nanostructured-TiO2 thin films prepared by sol-gel technique

In this paper we report on the effect of annealing on the microsctructural and optoelectronic properties of titanium dioxide (TiO₂) thin films prepared using sol-gel method onto silicon (Si) (100) and quartz substrates. The annealing temperatures range from 200 to 1000 °C. The Microstructural properties of annealed thin films were investigated by Thermal gravimetric analyses (TGA), X-ray diffraction (XRD) and Raman Spectroscopy. The surface morphology of the film was examined using Atomic Force Microscopy (AFM) method. The optical properties of TiO₂ thin films were characterized using UV-VIS and Spectroscopic ellipsometry. The results have shown that the TiO₂ thin films persist in the anatase phase even after annealing at 800 °C. The phase transformation from anatase to rutile occurred only when the films were annealed at 1000 °C. AFM studies revealed nanocrystalline structure where their shape and density depend strongly on the annealing temperatures. The elaborated nanostructured-TiO₂ thin films present a high transparency in the visible range. Spectroscopic ellipsometry (SE) study was used to determine the effect of annealing temperature on the thickness and on the optical constant of TiO₂ thin films. Spectroscopic ellipsometry and UV-VIS shows that the band gap of TiO₂ thin films was found to decrease when the annealing temperature increases. The Anatase phase was find to show higher photocatalytic activity than the rutile one.