Electronic structure and self-assembling processes in platinum metalloporphyrins: photoemission and AFM studies

The main goal of this paper is to investigate the electronic structure of valence band and core levels as well as surface topography of pristine tetraphenylporphyrin and Pt-based compounds Pt-TPP(p-COOH₃)₄, Pt-TPP(m-OCH₃)₄, PtCl₂-TPP(m-OCH₃)₄ thin films. The electronic structure of various Pt-based metalloporphyrins which were investigated in dependence on their chemical structure and spectra were measured by high-resolution X-ray photoelectron spectroscopy (XPS) of valence band and Pt4f, Pt4d, C1s, O1s, N1s core levels. Results of atomic force microscopy (AFM) studies of topography and self-assembling processes in thin films of porphyrines are presented and discussed.     

Surface characteristics of Zinc–TiO2 coatings prepared via micro-arc oxidation

Titanium (Ti) and its alloys are widely used as metallic biomaterials for fabrication of dental and orthopedic implants due to their favorable biocompatibility and corrosion resistance in a body environment. However, the thin oxide layer (TiO₂) on Ti substrate formed naturally in air or in many aqueous environments is bioinert and surrounded by fibrous tissues without producing any chemical or biological bond to bone when implanted. In the present work, Zinc-incorporated porous TiO₂ coatings (Zn–TiO₂) were prepared on Ti substrate by micro-arc oxidation (MAO) technique in the zinc gluconate-containing electrolyte. The surface morphology, cross-sectional morphology, composition, and phase of the coatings were analyzed using scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffractometry, respectively. Surface topography and roughness of the coatings were investigated by atomic force microscopy operated in tapping mode. The results showed that Zn was successfully incorporated into the porous TiO₂ coatings, which did not alter apparently its surface topography and phase composition. In conclusion, the formation of porous Zn–TiO₂ coatings endow Ti with potential bioactivity and antibacterial activity, and we believe that the porous Zn–TiO₂ coatings on Ti by MAO technique might be promising candidates for orthopedic and dental implants     

On the effects of using CO2 and F2 lasers to modify the wettability of a polymeric biomaterial

Enhancement of the surface properties of a material by means of laser radiation has been amply demonstrated previously. In this work a comparative study for the surface modification of nylon 6,6 has been conducted in order to vary the wettability characteristics using CO₂ and excimer lasers. This was done by producing 50 μm spaced (with depths between 1 and 10 μm) trench-like patterns using various laser parameters such as varying the laser power for the CO₂ laser and number of pulses for the excimer laser. Topographical changes were analysed using optical microscopy and white light interferometry which indicated that both laser systems can be implemented for modifying the topography of nylon 6,6. Variations in the surface chemistry were evaluated using energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy analysis which showed that the O₂ increased by up to 1.5 at% and decreased by up to 1.6 at% for the CO₂ and F₂ laser patterned samples, respectively. Modification of the wettability characteristics was quantified by measuring the advancing contact angle, which was found to increase in all instances for both laser systems. Emery paper roughened samples were also analysed in the same manner to determine that the topographical pattern played a major role in the wettability characteristics of nylon 6,6. From this, it is proposed that the increase in contact angle for the laser processed samples is due to a mixed intermediate state wetting regime owed to the periodic surface roughness brought about by the laser-induced trench-like topographical patterns.     

Microstructure of a composite with a quasicrystalline phase fraction obtained by directional solidification of Al61Cu27Fe12 alloy

The microstructure of a composite containing a quasicrystal phase, i.e. so-called crystal–quasicrystal (CQ) composite, was studied. The CQ composite was obtained by the Bridgman method via solidification of Al₆₁Cu₂₇Fe₁₂ alloy (numbers indicate at%). The process was conducted at a pull out rate of v = 0.07 mm/min. The average temperature gradient in the heating zone was 43 K/cm. The composite matrix consisted of cubic β phase Al(Fe, Cu), with reinforcement of λ-phase rod-shaped fibres surrounded by a quasicrystal icosahedral ψ phase, which also existed in the fibre core. The fibres were rhomboidal in cross-section. The composite was studied using X-ray and electron diffraction, light-optical and scanning electron microscopy (SEM), X-ray topography and Laue diffraction.     

MAO-synthesized Al2O3-supported V2O5 nano-porous catalysts: Growth, characterization, and photoactivity

V₂O₅-loaded Al₂O₃ layers were successfully grown via micro-arc oxidation (MAO) process for the first time. Surface morphology and topography of the layers were investigated by scanning electron microscope (SEM) and atomic force microscope (AFM). It was found that the composite layers had a porous structure with a rough surface which is suitable for catalytic applications. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and energy dispersive X-ray spectroscopy (EDS) techniques were also employed to study phase structure and chemical composition of the composite layers. The layers consisted of γ-alumina, α-alumina, and vanadium pentoxide phases in which their relative contents varied with the applied voltage. Meanwhile, optical properties of the composite layers were investigated using UV-vis spectrophotometry technique, and the band gap energy was calculated as 3.15 eV. Furthermore, photocatalytic performance of the synthesized composite layers was determined by measuring the decomposition rate of methylene blue solution, as a model compound, on the surface of the layers under ultra violet photo-irradiation. It was found that more than 91% of the methylene blue was degraded after 120 min with a rate constant of k = 0.0192 min⁻¹.     

Piezoelectric La3Ga5.3Ta0.5Al0.2O14 crystal: growth,crystal structure perfection,piezoelectric, and acoustic properties

A five-component crystal of lanthanum–gallium silicate group La₃Ga_5.3Ta_0.5Al_0.2O₁₄ (LGTA) was grown by the Czochralski method. The LGTA crystal possesses unique thermal properties and substitution of Al for Ga in the unit cell leads to a substantial increase of electrical resistance at high temperatures. The unit cell parameters of LGTA were determined by powder diffraction. X-ray topography was used to study the crystal structure perfection: the growth banding normal to the growth axis were visualized. The independent piezoelectric constants d ₁₁ and d ₁₄ were measured by X-ray diffraction in the Bragg and Laue geometries. Excitation and propagation of surface acoustic waves were studied by the double-crystal X-ray diffraction at the BESSY II synchrotron radiation source. The analysis of the diffraction spectra of acoustically modulated crystals permitted the determination of the velocity of acoustic wave propagation and the power flow angles in different acoustic cuts of the LGTA crystal.     

Pulsed laser deposition of semiconducting crystalline double-doped barium titanate thin films on nickel substrates

We synthesized by pulsed laser deposition (Ba,Sr,Y)TiO₃ and (Ba,Pb,Y)TiO₃ thin films on mechanically polished nickel substrates.The synthesized thin films were analyzed for: crystalline structure by X-ray diffractometry, morphology and surface topography by atomic force microscopy, optical and scanning electron microscopy, and elemental composition by energy dispersive X-ray spectroscopy and electrical properties by electrical measurements.We have shown that film properties were determined by the dopants, target composition, and deposition parameters (oxygen pressure, substrate temperature and incident laser fluence). All films exhibited a semiconducting behavior, as proved by the decrease of electrical resistance with heating temperature.     

Study of the specific features of lithium niobate crystals near the domain walls

The domain walls in LiNbO₃ are studied using X-ray topography, X-ray diffraction, and scanning electron microscopy. It is shown that the regions of distortions of the crystal lattice near the domain walls of different types are different and have lateral sizes of 100–200 μm. The character and the magnitude of the distortions are substantially dependent on the method of formation of the domain structure. Under irradiation in a scanning electron microscope, the crystal region up to 25 μm in width near the “tail-to-tail” domain walls is charged more slowly and, unlike the “head-to-head” domain walls, exhibits a dynamic charge image in the secondary-electron regime.     

Formation of gold nanoparticles in heat-treated reactive co-sputtered Au-SiO2 thin films

In this work, formation of gold nanoparticles in radio frequency (RF) reactive magnetron co-sputtered Au-SiO₂ thin films post annealed at different temperatures in Ar + H₂ atmosphere has been investigated. Optical, surface topography, chemical state and crystalline properties of the prepared films were analyzed by using UV-visible spectrophotometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) techniques, respectively. Optical absorption spectrum of the Au-SiO₂ thin films annealed at 800 °C showed one surface plasmon resonance (SPR) absorption peak located at 520 nm relating to gold nanoparticles. According to XPS analysis, it was found that the gold nanoparticles had a tendency to accumulate on surface of the heat-treated films in the metallic state. AFM images showed that the nanoparticles were uniformly distributed on the film surface with grain size of about 30 nm. Using XRD analysis average crystalline size of the Au particles was estimated to about 20 nm.     

单晶Si表面离子束溅射沉积Co纳米薄膜的研究

采用离子束溅射沉积法，在单晶Si基片上制备了不同厚度(1—100nm)的Co纳米薄膜.利用原子力显微镜、X射线光电子能谱(XPS)仪和X射线衍射仪对不同厚度的Co纳米薄膜进行了分析和研究.结果表明：当薄膜厚度为1—10nm时，沉积颗粒形态随薄膜厚度增加将由二维生长的细长胞状过渡到多个颗粒聚集成的球状.当膜厚大于10nm时，小颗粒球聚集成大颗粒球，颗粒球呈现三维生长状态.表面粗糙度随膜厚的增加呈现先增加后减小的趋势，在膜厚为3nm时出现极值.XPS全程宽扫描和窄扫描显示：薄膜表面的元素成分为Co，化学态分别 关键词： 离子束沉积 纳米薄膜 X射线光电子能谱 X射线衍射     

Advanced piezoelectric crystal Ca3TaGa3Si2O14: growth,crystal structure perfection,and acoustic properties

A five-component crystal of the lanthanum–gallium silicate family Ca₃TaGa₃Si₂O₁₄ (CTGS) was grown by the Czochralski method. The CTGS crystal, like the langasite crystal (La₃Ga₅SiO₁₄, LGS), possesses unique temperature properties and the fewer number of the Ga atoms in the unit cell makes the density much lower and, consequently, increases the velocity of acoustic wave propagation. The unit-cell parameters were determined by the powder diffraction technique. The defects in the CTGS crystal structure were studied by X-ray topography, which enables the visualization of growth banding characteristics of crystals grown by the Czochralski method. Surface acoustic wave (SAW) propagation in the CTGS crystal was investigated by the high-resolution X-ray diffraction method on the BESSY II synchrotron radiation source. The velocities of propagation and power flow angles of SAWs in the Y- and X-cuts of the CTGS crystal were determined from the X-ray diffraction spectra.     

直拉硅单晶原生微缺陷的观察

对沿<100>方向生长的p型和沿<111>方向生长的n型宏观无位错直拉硅单晶,用铜缀饰X射线形貌术和腐蚀法观察到两种不同类型的微缺陷,对n型硅单晶还观察到一种特殊组态的微缺陷。对观察到的微缺陷的分布、组态进行了初步的分析。本文首次采用X射线透射投影和截面形貌术对硅单晶原生微缺陷进行直接观察,获得了相应的微缺陷图。所观察到的微缺陷的组态、尺度、分布等与铜缀饰X射线透射形貌图所示结果一致。 关键词：     

Investigation into the structural perfection and acoustic properties of a piezoelectric Ca3TaGa3Si2O14 crystal

Ca₃TaGa₃Si₂O₁₄ (CTGS) crystals are a new promising material from the lanthanum-gallium silicate family, which can be employed in high-temperature sensors and other acoustoelectronic devices. The structural perfection and acoustic properties of CTGS crystals have been investigated via X-ray topography and diffractometry at the BESSY II synchrotron radiation source in the geometry of a double-crystal X-ray diffractometer.     

Surface modification of pure titanium by hydroxyapatite-containing composite coatings

Micro-arc oxidation (MAO) is commonly applied to modify the surface of titanium (Ti)-based medical implants with a bioactive and porous Ti oxide (TiO₂) coating. The study reports a new method of incorporating hydroxyapatite (HA) within the TiO₂ coating by MAO and alkali heat treatment (AHT) in the solution containing Ca ion and P ion. The morphology, composition and phase composition of the coatings were analyzed with scanning electron microscopy with energy-dispersive X-ray spectrometer and X-ray diffraction. Surface topography and roughness of the coatings were investigated by atomic force microscopy operated in the tapping mode. The results showed that TiO₂-based coatings were obtained on pure Ti by MAO with an electrolyte containing Ca ion and P ion; the prepared MAO coatings were mainly composed of Ca, P, O and Ti. AHT transformed Ca and P to HA crystals. In conclusion, the TiO₂/HA composite coatings can be obtained on the surface of pure Ti by MAO and AHT, and the addition of Ca ion and P ion to the AHT solution contributed to the formation of HA.     

Formation of nano-hillocks by impact of swift heavy ions on thin films of TiO2

Amorphous thin films of TiO₂ are irradiated by swift heavy ion (SHI) beam. Surface topography is studied by atomic force microscopy (AFM). Formation of nanosized oblate hillocks on the surface of irradiated films is investigated by AFM studies. After irradiation, amorphous to crystalline phase transition is observed in glancing angle X-ray diffraction (GAXRD) and Raman spectroscopy studies. Photoluminescence (PL)-spectroscopy is carried out for optical characterization. Threshold value necessary for emergence of hillocks is estimated.     

The influence of moisture on atmospheric pressure plasma etching of PA6 films

The moisture in the substrate material may have a potential influence on atmospheric pressure plasma treatment. In order to investigate how the existence of moisture affects atmospheric pressure plasma treatment, polyamide 6 (PA6) films were treated by helium, helium/oxygen (O₂) plasmas using atmospheric pressure plasma jet (APPJ) at different moisture regain. The film surfaces were investigated using contact-angle measurements, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) to characterize the surfaces. The exposure of PA6 film surfaces to the plasmas led to the etching process on the surfaces and changes in the topography of the surfaces. It was shown that the etching rate and the surface roughness were higher for the 9.33% moisture regain (relative humidity 100%) group than that of the 1.61% moisture regain (relative humidity 10%) group with the same plasma gas and power.     

On the generation of bulk microdefects in phosphorus-diffused monocrystalline silicon solar wafers after a high-thermal treatment studied by X-ray topography

Oxygen is the most important impurity in free dislocation Czochralski silicon single crystals incorporated interstitially during the growth. The knowledge of oxygen behavior after thermal processes is of great technological importance, since different kinds of bulk microdefects such us SiO₂ precipitates, dislocation loops and stacking faults can be generated. In monocrystalline silicon solar cell manufacturing fabrication, there are several high-thermal treatments. The first is the diffusion process at 850–900 °C. Three different kinds of phosphorus diffusion wafers, standard PO₃Cl liquid, spray-on and screen printing, were comparatively studied by X-ray topography showing that phosphorus diffusion improves the crystal quality by a gettering process whose best efficiency is in PO₃Cl-diffused wafers. Later, another fabrication high-thermal step is for instance the rear surface passivation taking place at temperatures from 800 to 1,050 °C. For this reason, it is important to study how a high-thermal treatment at 1,000 °C affects the different phosphorus-diffused wafers mentioned above. To evaluate and characterize the possible defects induced by the oxygen precipitation, X-ray topography has been employed. Results show that annealed wafers are not perfect crystals; the oxygen precipitation induces the generation of bulk microdefects whose kind, size and density depend on the diffusion method employed. In PO₃Cl and spray-on diffused wafers, retardation in the oxygen precipitation process takes place after annealing, while in screen printing this process is recovered and a kind of mixed defects between dislocation loops and platelet precipitates is generated.     

Structural and compositional mapping of a phase-separated Langmuir–Blodgett monolayer by X-ray photoelectron emission microscopy

The structure and composition of phase-separated Langmuir–Blodgett monolayer films comprised of mixtures of arachidic acid (C₁₉H₃₉COOH) and perfluorotetradecanoic acid (C₁₃F₂₇COOH) were characterized using a combination of X-ray photoelectron emission microscopy (X-PEEM), secondary electron emission microscopy (SEEM) and atomic force microscopy (AFM). X-PEEM provides high lateral spatial resolution and is directly sensitive to the elemental and chemical (functional group) composition of these ultrathin films through the chemical sensitivity of NEXAFS spectroscopy; AFM provides high-resolution imaging, both in terms of lateral and vertical (height) film topography. SEEM provides additional structural and electronic information through work function and electron scattering effects. The combination is used for chemical mapping of the phase-separated domains in the monolayer film. Our results directly confirm previous AFM measurements that suggested that the discontinuous domains are enriched in arachidic acid, whereas the surrounding continuous domain is a mixture of both arachidic acid and perfluorotetradecanoic acid.     

Structural and magnetic properties of cadmium substituted Ni-Al ferrites

Nickel Cadmium Aluminum Ferrites with the general formula Ni_1−xCd_xAl_0.6Fe_1.4O₄ where x=0, 0.25, 0.50 and 0.75 were prepared through standard double sintering reaction method. The crystallography, surface morphology and magnetic properties were studied by X-ray diffractometer (XRD), Scanning Electron Microscope (SEM) and Vibrating Sample Magnetometer (VSM), respectively. The expected single phase spinel structure was confirmed by XRD analysis. Lattice parameter and X-ray density were increased monotonically by increasing Cd concentration due to the larger ionic radii of the cadmium ion. Surface topography of the samples consists of fine cubical shape microstructures. The average grain size increased with increase in cadmium concentration. The saturation magnetization was found to be increased with increase in cadmium content up to x=0.50 and then decreased with further increasing cadmium concentration for x=0.75.     

LiNbO3晶体中包裹物和位错的X射线形貌研究

用X射线透射扫描形貌方法研究了LiNb0₃晶体中的包裹物和位错。在实验中发现了包裹物的相应于不同衍射矢量的X射线形貌与基于各向同性理论预言的形貌之间存在分歧,这被解释为弹性各向异性效应。同时还观察到Burgers矢量为最短点阵平移矢量1/3的纯刃型位错和次短点阵平移矢量1/3<0111>的纯螺型位错,以及由该螺型位错组成的纯扭转晶界。 关键词：