Structural transition of ZnO thin films produced by RF magnetron sputtering at low temperatures

Zinc oxide (ZnO) thin films were prepared using reactive radio-frequency magnetron sputtering of a pure metallic zinc target onto glass substrates. The evolution of the surface morphology and the optical properties of the films were studied as a function of the substrate temperature, which was varied from 50 to 250 C. The surface topography of the samples was examined using atomic force microscopy (AFM), and their optical properties were studied via transmittance measurements in the UV-Vis-NIR region. DRX and AFM analyses showed that the surface morphology undergoes a structural transition at substrate temperatures of around 150 C. Actually, at 50 C the formation of small grains was observed while at 250 C the grains observed were larger and had more irregular shapes. The optical gap remained constant at ∼3.3 eV for all films. In the visible region, the average optical transmittance was 80 %. From these results, one can conclude that the morphological properties of the ZnO thin films were more greatly affected by the substrate temperature, due to mis-orientation of polycrystalline grains, than were the optical properties. © 2013 Springer Science+Business Media New York.

Local Electrochemical Investigation of Single Grains of Polycrystalline Cu-16%Zn-8%Al Alloy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

High vacuum tribology of polycrystalline diamond coatings

Polycrystalline diamond coatings have been grown on unpolished side of Si(100) wafers by hot filament chemical vapour deposition process. The morphology of the grown coatings has been varied from cauliflower morphology to faceted morphology by manipulation of the growth temperature from 700 degrees C to 900 degrees C and methane gas concentration from 3% to 1.5%. It is found that the coefficient of friction of the coatings under high vacuum of 133.32 x 10(-7) Pa (10(-7) torr) with nanocrystalline grains can be manipulated to 0.35 to enhance tribological behaviour of bare Si substrates.

Size Effects on Strength in the Transition from Single-to-Polycrystalline Behavior

During the transition from single crystalline to polycrystalline behavior, the available data show the strength increasing or decreasing as the number of grains in a cross section is reduced. Tensile experiments were conducted on polycrystalline Ni with grain sizes (d) between 16 and 140 mu m and varying specimen thickness (t), covering a range of lambda (-t/d) between similar to 0.5 and 20. With a decrease in lambda, the data revealed a consistent trend of strength being independent of lambda at large lambda, an increase in strength, and then a decrease in strength. Microstructural studies revealed that lower constraints enabled easier rotation of the surface grains and texture evolution, independent of the specimen thickness. In specimen interiors, there was a greater ease of rotation in thinner samples. Measurements of misorientation deviations within grains revealed important differences in the specimen interiors. A simple model is developed taking into account the additional geometrically necessary dislocations due to variations in the behavior of surface and interior grains, leading to additional strengthening. A suitable combination of this strengthening and surface weakening can give rise to wide range of possibilities with a decrease in lambda, including weakening, strengthening, and strengthening and weakening.

A meso elastoplastic constitutive model for polycrystalline metals based on equivalent slip systems with latent hardening

A meso material model for polycrystalline metals is proposed, in which the tiny slip systems distributing randomly between crystal slices in micro-grains or on grain boundaries are replaced by macro equivalent slip systems determined by the work-conjugate principle. The elastoplastic constitutive equation of this model is formulated for the active hardening, latent hardening and Bauschinger effect to predict macro elastoplastic stress-strain responses of polycrystalline metals under complex loading conditions. The influence of the material property parameters on size and shape of the subsequent yield surfaces is numerically investigated to demonstrate the fundamental features of the proposed material model. The derived constitutive equation is proved accurate and efficient in numerical analysis. Compared with the self-consistent theories with crystal grains as their basic components, the present theory is much simpler in mathematical treatment.

An anisotropic elastic-plastic constitutive model for single and polycrystalline metals .1. Theoretical developments

An anisotropic elastic-plastic constitutive model for single and polycrystalline metals is proposed. The anisotropic hardening of single crystals, at first, is discussed with the viewpoint of yield surface and a new formulation of it is proposed. Then, a model for the anisotropic hardening of polycrystals is suggested by increasing the number of slip systems and incorporating the interaction of all slip systems. The interaction of grains through grain boundaries is shown to be similar to, and incorporated into, the interaction of slip systems in grains. The numerical predictions and their comparisons with experiments will follow in Part II of this paper.

Bundles of polytwins as meta-elastic domains in the thin polycrystalline simple multi-ferroic system PZT.

We used enhanced piezo-response force microscopy (E-PFM) to investigate both ferroelastic and ferroelectric nanodomains in thin films of the simple multi-ferroic system PbZr(0.3)Ti(0.7)O(3) (PZT). We show how the grains are organized into a new type of elastic domain bundles of the well-known periodic elastic twins. Here we present these bundle domains and discuss their stability and origin. Moreover, we show that they can arrange in such a way as to release strain in a more effective way than simple twinning. Finally, we show that these bundle domains can arrange to form the macroscopic ferroelectric domains that constitute the basis of ferroelectric-based memory devices.

Discrete dislocation plasticity analysis of crack-tip fields in polycrystalline materials

Small scale yielding around a mode I crack is analysed using polycrystalline discrete dislocation plasticity. Plane strain analyses are carried out with the dislocations all of edge character and modelled as line singularities in a linear elastic material. The lattice resistance to dislocation motion, nucleation, interaction with obstacles and annihilation are incorporated through a set of constitutive rules. Grain boundaries are modelled as impenetrable to dislocations. The polycrystalline material is taken to consist of two types of square grains, one of which has a bcc-like orientation and the other an fcc-like orientation. For both orientations there are three active slip systems. Alternating rows, alternating columns and a checker-board-like arrangement of the grains is used to construct the polycrystalline materials. Consistent with the increasing yield strength of the polycrystalline material with decreasing grain size, the calculations predict a decrease in both the plastic zone size and the crack-tip opening displacement for a given applied mode I stress intensity factor. Furthermore, slip-band and kink-band formation is inhibited by all grain arrangements and, with decreasing grain size, the stress and strain distributions more closely resemble the HRR fields with the crack-tip opening approximately inversely proportional to the yield strength of the polycrystalline materials. The calculations predict a reduction in fracture toughness with decreasing grain size associated with the grain boundaries acting as effective barriers to dislocation motion.

Nucleation, growth, and control of ferroelectric-ferroelastic domains in thin polycrystalline films

The unique response of ferroic materials to external excitations facilitates them for diverse technologies, such as nonvolatile memory devices. The primary driving force behind this response is encoded in domain switching. In bulk ferroics, domains switch in a two-step process: nucleation and growth. For ferroelectrics, this can be explained by the Kolmogorov-Avrami-Ishibashi (KAI) model. Nevertheless, it is unclear whether domains remain correlated in finite geometries, as required by the KAI model. Moreover, although ferroelastic domains exist in many ferroelectrics, experimental limitations have hindered the study of their switching mechanisms. This uncertainty limits our understanding of domain switching and controllability, preventing thin-film and polycrystalline ferroelectrics from reaching their full technological potential. Here we used piezoresponse force microscopy to study the switching mechanisms of ferroelectric-ferroelastic domains in thin polycrystalline Pb 0.7Zr0.3TiO3 films at the nanometer scale. We have found that switched biferroic domains can nucleate at multiple sites with a coherence length that may span several grains, and that nucleators merge to form mesoscale domains, in a manner consistent with that expected from the KAI model. © 2012 American Physical Society.

Host-sensitized luminescence of Dy3+, Pr3+, Tb3+ in polycrystalline SrIn2O4 for field emission displays

SrIn2O4:Dy3+/Pr3+/Tb3+ white/red/green phosphors were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), diffuse reflectance, photoluminescence, cathodoluminescence spectra, and lifetimes were utilized to characterize the samples. XRD reveal that the samples begin to crystallize at 800 degrees C and pure SrIn2O4 phase can be obtained at 900 degrees C. FE-SEM images indicate that the SrIn2O4:Dy3+, SrIn2O4:Pr3+, and SrIn2O4:Tb3+ samples consist of fine and spherical grains with size around 200-400 nm. Under the excitation of ultraviolet light and low-voltage electron beams (1 - 5 kV), the SrIn2O4:Dy3+, SrIn2O4: Pr3+, and SrIn2O4: Tb3+ phosphors show the characteristic emissions of Dy3+ (F-4(9/2) - H-6(15/2) at 492 nm and 4F(9/2) - 6H(13/2) at 581 nm, near white), Pr3+ (P-3(0) - H-3(4) at 493 nm, D-1(2) - H-3(4) at 606 nm, and P-3(0) - H-3(6) at 617 nm, red) and Tb3+ (D-5(4) - F-7(6,5,4,3) transitions dominated by D-5(4) - F-7(5) at 544 nm, green), respectively. All of the luminescence resulted from an efficient energy transfer from the SrIn2O4 host lattice to the doped Dy3+, Pr3+, and Tb3+ ions, and the luminescence mechanisms have been proposed.

Host-sensitized luminescence of Dy3+, Pr3+ , Tb3+ in polycrystalline CaIn2O4 for field emission displays

Caln(2)O(4):Dy3+/Pr3+/Tb3+ blue-white/green/green phosphors were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), diffuse reflectance, photoluminescence (PL) and cathodoluminescencc (CL) spectra as well as lifetimes were utilized to characterize the samples. The XRD results reveal that the samples begin to crystallize at 800 degrees C 3-1 and pure CaIn2O4 phase can be obtained after annealing at 900 degrees C. The FE-SEM images indicate that the CaIn2O4:Dy3+, CaIn2O4:Pr3+ and CaIn2O4:Tb3+ samples consist of spherical grains with size around 200-400nm. Under the excitation of ultraviolet light and low electron beams (1-5kV), the CaIn2O4:Dy3+, CaIn2O4:Pr3+ and CaIn2O4:Tb3+ phosphors show the characteristic emissions of Dy3+ ((F9/2-H15/2)-F-4-H-6 and (F9/2-H13/2)-F-4-H-6 transitions, blue-white), Pr3+ ((P0-H4)-P-3-H-3, (D2-H4)-D-1-H-3 and (P1-H5)-P-3-H-3 transitions, green) and Tb3+ ((D4-F6,5,4,3)-D-5-F-7 transitions, green), respectively. All the luminescence is resulted from an efficient energy transfer from the CaIn2O4 host lattice to the doped Dy3+ ,Pr3+ and Tb3+ ions, and the corresponding luminescence mechanisms have been proposed.

Light emission from scanning tunnelling microscope on polycrystalline Au films - what is happening at the single-grain level?

When operated with a metallic tip and sample the scanning tunnelling microscope constitutes a nanoscale, plasmonic light source yielding broadband emission up to a photon energy determined by the applied bias. The emission is due to tunnelling electron excitation and subsequent radiative decay of localized plasmon modes, which can be on the lateral scale of a single metal grain (similar to 25 nm) or less. For a Au-tip/Au-polycrystalline sample under ambient conditions it is found that the intensity and spectral content of the emitted light are not dependent on the lateral grain dimension, but are predominantly determined by the tip geometry. However, the intensity increases strongly with increasing film thickness (grain depth) up to 20-25 nm or approximately the skin depth of the Au film. Photon maps can show less emissive grains and two classes of this occurrence are distinguished. The first is geometrical in origin - a double-tip structure in this case - while the second is due to a contamination-induced lowering of the local work function that causes the tunnel gap to increase. It is suggested that differences in work-function lowering between grains presenting different crystalline facets, combined with an exponential decay in emitted light intensity with tip - sample distance, leads to grain contrast. These results are relevant to tip-enhanced Raman scattering and the fabrication of micro/nano-scale planar, light-emitting tunnel devices.

In-situ white beam microdiffraction study of the deformation behavior in polycrystalline magnesium alloy during uniaxial loading

Scanning white beam X-ray microdiffraction has been used to study the heterogeneous grain deformation in a polycrystalline Mg alloy (MgAZ31). The high spatial resolution achieved on beamline 7.3.3 at the Advanced Light Source provides a unique method to measure the elastic strain and orientation of single grains as a function of applied load. To carry out in-situ measurements a light weight (~0.5kg) tensile stage, capable of providing uniaxial loads of up to 600kg, was designed to collect diffraction data on the loading and unloading cycle. In-situ observation of the deformation process provides insight about the crystallographic deformation mode via twinning and dislocation slip.

Evaluation of the effect of the stoichiometric ratio of Ca/Cu on the electrical and microstructural properties of the CaCu3Ti4O12 polycrystalline system

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)