Studies on solution-grown crystals of polyethylene terephthalate and some copolyesters. II. Physical properties of the solution-grown crystals add the hydrolyzed crystals

The viscoeiastic properties and the wide-line NMR spectra of solution-grown crystals and hydrolyzed crystals of polyethylene terephthalate and some copolyesters were measured. A new NMR narrowing and new viscoelastic absorption were observed at temperatures higher than that of the primary dispersion of the solution-grown crystals for all polymers cited above. It was clarified from the thermal expansion curve of the crystal lattice, as determined by X-ray diffraction, and from the crystallinity dependence of the absorption intensities that the new dispersion is caused by molecular motion in the crystalline region. The primary dispersion of the hydrolyzed crystals could scarcely be observed and only the narrowing corresponding to the crystalline dispersion was observed. This suggests that the loop region of the lamellar crystals was removed and the “pure” crystal was obtained.     

Influence of deposition conditions on the structural characteristics of sublimated CdTe thin films

In this paper the results obtained by X-ray diffraction studies on the structural characteristics of CdTe thin films deposited onto glass substrates by close-spaced sublimation technique are presented. Using different experimental arrangements and appropriate settings for growth parameters, the films with different polycrystalline structures were prepared. The geometry and the volume of the deposition chamber influence the size of film crystallites and also their preferential orientation. The role of deposition parameters such as the substrate temperature, the incidence angle, the film thickness, and the heat treatment in determination of the structural properties of the films are also investigated. Received: 26 November 1999 / Accepted: 7 January 2000 / Published online: 5 April 2000     

Characterization and Magnetic Properties of Iron-Based Alloy Antidot Arrays

Fe29Cerl and Fe19Ni81 antidot arrays, with different dimensions, are prepared with the rf magnetron sputtering method onto the porous alumina substrate. The size and shape of antidot arrays are characterized by scanning electron microscopy. The glancing angle x-ray diffraction patterns of Fe29C071 and FelgNi81 antidot arrays indicate the bcc and fcc structures, respectively. The coercivities of both the alloys show abnormal thickness dependence, which are discussed qualitatively by considering the pinning and the thickness effect to the films.     

Effect of thickness on structural, optical and electrical properties of nanostructured ZnO thin films by spray pyrolysis

Transparent conducting zinc oxide thin films were prepared by spray pyrolytic decomposition of zinc acetate onto glass substrates with different thickness. The crystallographic structure of the films was studied by X-ray diffraction (XRD). XRD measurement showed that the films were crystallized in the wurtzite phase type. The grain size, lattice constants and strain in films were calculated. The grain size increases with thickness. The studies on the optical properties show that the direct band gap value increases from 3.15 to 3.24 eV when the thickness varies from 600 to 2350 nm. The temperature dependence of the electrical conductivity during the heat treatment was studied. It was observed that heat treatment improve the electrical conductivity of the ZnO thin films. The conductivity was found to increase with film thickness.     

Thickness dependence and annealing effects on the reflectance of thin Cd,Ga and In films freshly deposited at 77 K

The reflectance of thin Cd, Ga and In films with various thicknesses is measured during isochronal annealing above 77 K, immediately after deposition. The irreversibility of temperature dependence of reflectance factor is related to annihilation of lattice defects, growth of crystallites and granulation.     

Al掺杂ZnO薄膜的厚度对其结构及磁学性能的影响

采用直流磁控共溅的方法在玻璃基底上制备了不同厚度的Al掺杂ZnO薄膜,并在真空和空气中分别退火.利用X射线衍射仪(XRD)和物理性能测量仪(PPMS)对系列薄膜的结构和磁性进行了表征.XRD结果显示:随着膜厚的增加,晶粒尺寸逐渐增大,薄膜的内应力逐渐减小.在空气退火的薄膜样品中观察到了室温的铁磁性,薄膜的饱和磁化强度M_s 随着膜厚的增加而增大,而矫顽力H_c却随着膜厚的增加而减小. 关键词： Al掺杂ZnO薄膜 薄膜厚度 应力 铁磁性     

Thermal expansion of the skeleton of chain molecules in polymer crystals

The expansion of the carbon skeleton of molecules in crystallites and the longitudinal contraction of the crystallite lattice in poly(ethylene) (PE) and poly(caproamide) (PCA) with an increase in the temperature are measured using IR and Raman spectroscopy and x-ray diffraction. The thermal expansion of the carbon skeleton due to transverse vibrations is theoretically calculated within the atomic chain model. The theoretical and experimental data on the thermal expansion of the carbon skeleton are in good agreement.     

In situ X-ray diffraction investigation of porous silicon strains induced by the freezing of a confined organic fluid

High resolution X-ray diffraction is used to perform an in situ measurement of the variations of the lattice parameter of the nanometer size crystallites of porous silicon, induced by the freezing of a confined organic fluid, dodecane. Two p⁺ type PS layers of 60 and 70% porosity are investigated, and the variations of their lattice parameter with the temperature (in the range 150–300 K) are measured. The experimental curves are discussed in relation with the results of a previous calorimetric study of the freezing of confined dodecane. We explain the observed strains by the presence of capillary stresses, that appear in the layer due to the formation of internal liquid-vapour meniscus during the freezing process of the confined fluid. Received 22 October 1999 and Received in final form 25 March 2000     

Synthesis and Characterization of Ag@TiO2 Core-shell Nanoparticles and TiO2 Nanobubbles

Ag@TiO₂ core-shell structured particles of nano-size dimensions have been successfully prepared via a one-step way, which has proved quite effective in procuring stable colloids. Transmission electron microscopy (TEM) was employed to characterize the core size and the shell thickness, which typically were 20~40 nm and ~2 nm, respectively. X-ray diffraction (XRD) indicated the existence of silver. Optical absorption dependence on core size and synthetic temperature has been explored by UV–Vis absorption spectroscopy. Finally, the interesting titanium dioxide nanobubbles with silver core leached out by a unique means, were studied, which consequently proved the core-shell structure of the prepared nanoparticles, confirming the TEM observation.     

Effect of annealing on the structure and morphology of nylon 6 fibers

Changes in the structure of nylon 6 fibers annealed in dry and wet atmospheres were studied by small-and wide-angle x-ray diffraction. In the presence of water or saturated steam, fibers can be annealed to the same strucutral state at temperatures 70°C lower than in dry atmosphere. This is due to the enhanced mobility of the molecular segments in the amorphous region, a mechanism which is also known to lower the T_g by the same amount. Upon annealing under unconstrained conditions, lamellar spacing, crystallite size in the equatorial plane, crystalline as well as fiber density, and the chain-axis repeat increase with annealing-temperature; whereas crystalline orientation and the Van der Waals separation of the hydrogen-bonded sheets decrease. The monoclinic angle 8 remains constant at 66.7° (σ = 0.3°) and might depend on the starting fiber rather than on the treatment of the fiber. Most of these changes occur above a critical temperature of 170°C if dry, or 100°C if wet; rate of crystallization is also the highest under these conditions in nylon. The effect of these changes on such fiber properties as dyeing and the role of micro voids in dye diffusion and in dye uptake are discussed. Surface premelting and the accompanying changes in the surface structure of the lamellae, selective melting, and more importantly, the longitudinal motion of the nylon 6 chains and the resulting folding of interfibrillar extended amorphous chains are invoked to explain the shrinkage of the fiber, disorientation of the crystallites, increase in crystalline perfection, and the increase in lamellar spacing.     

Influence of the quantum size effect for grazing electrons on the electronic conductivity of metal films

The thickness dependence of the electronic conductivity of thin (5–150 nm) single-crystal (100) films of refractory metals is investigated at different temperatures ranging from 4.2 K to room temperature. Regions of square-root, quasilinear, and quadratic dependences are observed. The quasilinear thickness dependence is explained by the influence of quantum effects on the transverse motion of electrons in the case when electron scattering by the film surfaces dominates. For macroscopic film thicknesses 30–50 nm, much greater than the Fermi wavelength of an electron, quantum corrections to the electronic conductivity reach values of the order of 50%. This is a consequence of the quantum size effect for grazing electrons, which leads to an anomaly in electron scattering by the film surfaces. The region of the quadratic thickness dependence corresponds to the quantum limit, and the square-root region corresponds to the classical limit. The effect is explained in a quasiclassical two-parameter model (the effective angle α* for small-angle electrons and the parameter γ, equal to the ratio of this angle to the diffraction angle) that takes into account the diffraction angular limits for grazing electrons. The effect occurs for parameters α*≪1 and γ∼1 and differs from the “ordinary” quantum size effect. Pis’ma Zh. éksp. Teor. Fiz. 66, No. 11, 693–698 (10 December 1997)     

Temperature dependent structure of spider silk by X-ray diffraction

We have investigated the structure of spider dragline silk by X-ray diffraction over a broad temperature range from room temperature up to thermal denaturation conditions. The dominating signal from the β-sheet crystallites is analyzed. Pronounced changes of scattering intensity starting at temperatures around 150 °C are observed. These changes are discussed in view of the respective lattice constants, crystal size, size distribution, crystallite number density and amino acid composition. PACS 87.68.+z; 87.15.-v; 87.64.Bx     

Synthesis and structural characterization of nanostructured copper

In this paper, we report on the preparation and characterization of nanocrystalline powder of copper by dc-magnetron sputtering. Liquid nitrogen cooled cold finger arrangement has been used to prepare nanocrystalline powder. The particle size, crystal structure, and morphology of the samples were characterized by in situ high temperature X-ray diffraction (XRD) and transmission electron microscope (TEM). Results of high temperature XRD showed that highly oriented (111) phase becomes randomly oriented at higher temperature with a systematic shift in peak positions toward lower 2θ values due to changes in lattice parameters. Temperature dependence of lattice constants under vacuum shows linear increase in their values. Diffraction patterns obtained from TEM are also in accordance with the XRD data.     

Study of titania nanorod films deposited by matrix-assisted pulsed laser evaporation as a function of laser fluence

The effects of annealing at 300 °C on gold nanostructures sputtered onto glass substrate were studied using XRD, SAXSees, the Van der Pauw method and ellipsometry. As-sputtered and annealed samples exhibit a different dependence of the gold lattice parameter on the sputtering time. With increasing sputtering time the average thickness of the layer and the size of gold crystallites increased. Another rapid enlargement of the crystallites is observed after annealing. The volume resistivity decreases rapidly with the increasing sputtering time for both, as-deposited and annealed structures. With increasing sputtering time initially discontinuous gold coverage changes gradually in a continuous one. Electrically continuous gold coverage on the as-sputtered and annealed samples exhibits the same concentration of free charge carriers and Hall mobility. Optical constants of as-deposited and annealed gold films determined by ellipsometry support resistivity measurements and clearly manifest the presence of plasmons in discontinuous films.     

Pressure dependence of the electric field gradient in the AgIn2 intermetallic compound

The pressure dependence of the electric field gradient (EFG) in the AgIn₂ intermetallic compound was measured from zero up to 35 kbar using the time differential perturbed angular correlation technique in¹¹¹Cd. The unit cell volume and thec/a ratio variations with pressure were measured up to 80 kbar. The temperature dependence of the cell parameters was also measured, in a range varying from 300 K up to 458 K. The relationship of these results showed that the contribution of the lattice thermal expansion to the EFG variations is about 1/3, a small but not negligible part. The estimated EFG volumetric dependence is at variance with the systematic results found in pure metals. Work supported in part by FINEP and CNPq (Brasil).     

Phonon dispersion in NiO

The phonon dispersion relations in NiO have been measured using coherent inelastic neutron diffraction. Good fits to the data were obtained using various shell models. The room temperature phonon density of states was calculated and used to determine the temperature dependence of the lattice specific heat and the Debye temperature.     

Frequency doubling of ultrashort pulses in a nonlinear photonic strontium tetraborate crystal

The second harmonic generation (SHG) of the femtosecond titanium-sapphire laser radiation was experimentally studied in the mode of nonlinear diffraction in the nonlinear photonic strontium tetraborate crystal. The spectrum of reciprocal lattice vectors of domain structures includes components responsible for the efficient frequency-tunable SHG in the spectral range of 355–510 nm. The maximum SHG efficiency was 1.9%. The SHG spectrum narrowing does not exceed 10–20%. The measured spectral dependence of the nonlinear diffraction angle is in good agreement with calculation.     

Holographic Bragg gratings in a photoresponsive cross-linked polymer-liquid-crystal composite

Holographic gratings were in a composite material that comprised a cross-linked polymer with azobenzene side chains and a nematic liquid crystal. Holographic recording was based on the photoinduced alignment of the nematic liquid crystal inside a cell as a result of amplification of the photoreorientation of azobenzene residues. The diffraction efficiency depends on cell thickness and reading angle of the gratings, so this composite material exhibits volume holographic properties with Bragg diffraction.     

Interfacial structure analysis of polymer laminate using SPring-8 X-ray microbeam

Interfacial structure of laminated polyethylene (PE)/polypropylene (PP) films was investigated by synchrotron X-ray microbeam. The X-ray microbeam (0.9 μm (vertical) × 1.7 μm (horizontal)) formed using a phase zone plate was irradiated on the cross-section of the laminated films. In order to irradiate X-ray microbeam in the direction perpendicular to the cross-section of the film sample, adjustment of the sample setting was performed by Thomson scattering method. The Thomson scattering intensity is proportional to the number of the irradiated electrons, so the irradiated position of the X-ray microbeam could be determined from the intensity profile with high spatial resolution. By changing the sample position, diffraction patterns could be obtained from the laminated films across the PE/PP interfacial region. The thickness of the interfacial region of the annealed laminate was estimated as 5 μm judging from the changes of the diffraction intensities from the PE crystallites to the PP ones. The interfacial thickness depended on the thermal treatment of the film. It was found that the adhesion strength of the PE/PP laminate increased with increasing the interfacial thickness. Both of PE and PP chains entangled each other during laminate processing. The entangled molecular chains play important role as anchoring effect at the PE/PP interdiffusion region. However, the phase separation progressed with further crystallization by annealing. Thus, the adhesion strength of the PE/PP laminate was considered to be influenced by the interfacial thickness.     

Fractal patterns on the onset of coherent structures in a coupled map lattice

We report the formation of Cantor set-like fractals during the development of coherent structures in a coupled map lattice (CML). The dependence of these structures on the size of the lattice as well as the first three dimensions of the associated fractal patterns are analyzed numerically.