Domain Bundle Boundaries in Single Crystal BaTiO3 Lamellae: Searching for Naturally Forming Dipole Flux-Closure / Quadrupole Chains

Naturally occurring boundaries between bundles of 90o stripe domains, which form in BaTiO3 lamellae on cooling through the Curie Temperature, have been characterised using both piezoresponse force microscopy (PFM) and scanning transmission electron microscopy (STEM). Detailed interpretation of the dipole configurations present at these boundaries (using data taken from PFM) shows that, in the vast majority of cases, they are composed of simple zigzag 180° domain walls. Topological information from STEM shows that, occasionally, domain bundle boundaries can support chains of dipole flux closure and quadrupole nanostructures, but these kinds of boundaries are comparatively rare; when such chains do exist, it is notable that singularities at the cores of the dipole structures are avoided. The symmetry of the boundary shows that diads and centres of inversion exist at positions where core singularities should have been expected.

Scaling of Superdomain Bands in Ferroelectric Dots

Bundles of 90° stripe domains have been observed to form into distinct groups, or bands, in mesoscale BaTiO3 single crystal dots. Vector piezoresponse force microscopy (PFM) shows that each band region, when considered as a single entity, possesses a resolved polarization that lies approximately along the pseudocubic direction; antiparallel alignment of this resultant polarization in adjacent bands means that these regions can be considered as 180° “superdomains.” For dots with sidewall dimensions below ~2 microns, Landau–Kittel like scaling in the width of these superdomains was observed, strongly suggesting that they form in response to lateral depolarizing fields. In larger dot structures, scaling laws break down. We have rationalized these observations by considering changes in the driving force for the adoption of equilibrium superdomain periodicities implied by Landau–Kittel-free energy models; we conclude that the formation of ordered bands of superdomains is a uniquely meso/nanoscale phenomenon. We also note that the superdomain bands found by PFM imaging in air contrast with the quadrant arrangements seen previously by Schilling et al. (Nano Lett., 9, 3359 (2009)) through transmission electron microscopy imaging in vacuum. The importance of the exact nature of the boundary conditions in determining the domain patterns that spontaneously form in nanostructures is therefore clearly implied.

Structural investigations and magnetic properties of sol-gel Ni0.5Zn0.5Fe2O4 thin films for microwave heating

Nanocrystalline Ni0.5Zn0.5Fe2O4 thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology, magnetic, and microwave absorption properties of the films calcined in the 673-1073 K range were studied with x-ray diffraction, scanning electron microscopy, x-ray photoelectron spectroscopy, atomic force microscopy, vibrating sample magnetometry, and evanescent microwave microscopy. All films were uniform without microcracks. Increasing the calcination temperature from 873 to 1073 K and time from 1 to 3 h resulted in an increase of the grain size from 12 to 27 nm. The saturation and remnant magnetization increased with increasing the grain size, while the coercivity demonstrated a maximum near a critical grain size of 21 nm due to the transition from monodomain to multidomain behavior. The complex permittivity of the Ni-Zn ferrite films was measured in the frequency range of 2-15 GHz. The heating behavior was studied in a multimode microwave cavity at 2.4 GHz. The highest microwave heating rate in the temperature range of 315-355 K was observed in the film close to the critical grain size.

Domain annihilation due to temperature and thickness gradients in single-crystal BaTiO3

The manner in which 90? ferroelectric-ferroelastic domains respond to changes in temperature has been mapped in BaTiO3 single crystals using atomic force microscopy. Domain periodicity remains unaltered until approximately 2 ? C below the Curie temperature (TC ), whereupon domains coarsened dramatically. This behavior was successfully rationalized by considering the temperature dependence of the parameters associated with standard models of ferroelastic domain formation. However, while successful in describing the expected radical increase in equilibrium period with temperature, the model did not predict the unusual mechanism by which domain coarsening occurred; this was not continuous at a local level but instead involved discrete domain annihilation events. Subsequent insights from a combination of free energy analysis for the system and further experimental data from an analogous situation, in which domain period increases with increasing crystal thickness, suggested that domain annihilation is inevitable whenever a component of the relevant gradient that affects domain period is orientated parallel to the domain walls. Consistent with this thesis, we note that, for the observations presented herein, the thermal gradient possessed a significant component parallel to the domain walls. We suggest that domain annihilation is a general feature of domain structures in gradient fields.

Characterization of novel Ag on TiO2 films for surface-enhanced Raman scattering

Novel Ag on TiO₂ films are generated by semiconductor photocatalysis and characterized by ultraviolet-visible (UV/Vis) spectroscopy, scanning electron microscopy (SEM), and atomic force microscopy (AFM), as well as assessed for surface-enhanced Raman scattering (SERS) activity. The nature and thickness of the photodeposited Ag, and thus the degree of SERS activity, is controlled by the time of exposure of the TiO₂ film to UV light. All such films exhibit the optical characteristics (λ_max ≅ 390 nm) of small (<20 nm) Ag particles, although this feature becomes less prominent as the film becomes thicker. The films comprise quite large (>40 nm) Ag islands that grow and merge with increasing levels of Ag photodeposition. Tested with a benzotriazole dye probe, the films are SERS active, exhibiting activity similar to that of 6-nm-thick vapordeposited films. The Ag/TiO₂ films exhibit a lower residual standard deviation (∼25%) compared with Ag vapor-deposited films (∼45%), which is, however, still unacceptable for quantitative work. The sample-to-sample variance could be reduced significantly (<7%) by spinning the film during the SERS measurement. The Ag/TiO₂ films are mechanically robust and resistant to removal and damage by scratching, unlike the Ag vapor-deposited films. The Ag/TiO₂ films also exhibit no obvious loss of SERS activity when stored in the dark under otherwise ambient conditions. The possible extension of this simple, effective method of producing Ag films for SERS, to metals other than Ag and to semiconductors other than TiO₂, is briefly discussed. 

Modification of biomaterial surface characteristics by body fluids in vitro

In practice, polyvinyl chloride endotracheal tubes and polyurethane urinary catheters are located in areas where they are exposed to the conditioning fluids saliva and urine, respectively. Samples of both biomaterials were incubated in these conditioning fluids and, following treatment, dynamic contact angle measurement and surface roughness assessment by atomic force microscopy were used to analyse surface characteristics. Over a 24 h period of contact with the conditioning fluids, the surface of both materials became significantly more hydrophilic (p

The potential of electron beam radiation for simultaneous surface modification and bioresorption control of PLLA

Bioresorbable polymers have been widely investigated as materials exhibiting significant potential for successful application in the fields of tissue engineering and drug delivery. Further to the ability to control degradation, surface engineering of polymers has been highlighted as a key method central to their development. Previous work has demonstrated the ability of electron beam (e-beam) technology to control the degradation profiles and bioresorption of a number of commercially relevant bioresorbable polymers (poly-l-lactic acid (PLLA), Llactide/DL-lactide co-polymer (PLDL) and poly(lactic-co-glycolic acid (PLGA)). This work investigates the further potential of ebeam technology to impart added biofunctionality through the manipulation of polymer (PLLA) surface properties. PLLA samples were subjected to e-beam treatments in air, with varying beam energies and doses. Surface characterization was then performed using contact angle analysis, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and atomic force microscopy. Results demonstrated a significant increase in surface wettability post e-beam treatment. In correlation with this, XPS data showed the introduction of oxygen-containing functional groups to the surface of PLLA. Raman spectroscopy indicated chain scission in the near surface region of PLLA (as predicted). However, e-beam effects on surface properties were not shown to be dependent on beam energy or dose. E-beam irradiation did not seem to affect the surface roughness of PLLA as a direct consequence of the treatment.

Regular nanodomain vertex arrays in BiFeO3 single crystals

Domain patterns consisting of triangular nanodomains of less than 50 nm size, arranged into long regular vertex arrays separated by stripe domains, were observed by (scanning and high-resolution) transmission electron microscopy and piezoresponse force microscopy in BiFeO3 single crystals grown from solution flux. Piezoresponse force microscopy analysis together with crystallographic analysis by selected area and nanobeam electron diffraction indicate that these patterns consist of ferroelectric 109 degrees domains. A possibility for conserving Kittel's law is discussed in terms of the patterns being confined to the skin layer observed recently on BiFeO3 single crystals.

Domain Bundle Boundaries in Single Crystal BaTiO3 Lamellae: Searching for Naturally Forming Dipole Flux-Closure/Quadrupole Chains

Naturally occurring boundaries between bundles of 90° stripe domains, which form in BaTiO3 lamellae on cooling through the Curie Temperature, have been characterized using both piezoresponse force microscopy (PFM) and scanning transmission electron microscopy (STEM). Detailed interpretation of the dipole configurations present at these boundaries (using data taken from PFM) shows that in the vast majority of cases they are composed of simple zigzag 180° domain walls. Topological information from STEM shows that occasionally domain bundle boundaries can support chains of dipole flux closure and quadrupole nanostructures, but these kinds of boundaries are comparatively rare; when such chains do exist, it is notable that singularities at the cores of the dipole
structures are avoided. The symmetry of the boundary shows that diads and centers of inversion exist at positions where core singularities should have been expected.

Polycrystalline silicon film growth in a SiF4/SiH4/H2 plasma

The growth of polycrystalline silicon (polysilicon) films from SiF4/SiH4/H2 gas mixtures is reported. The polysilicon films have been deposited in a multi process reactor by a PECVD process. The effect of r.f. power, chamber temperature and gas flow ratios on grain size and deposition rate have been determined. The fluorine concentration and the grain sizes of the films have been determined by SIMS and atomic force microscopy (AFM), respectively. Grain sizes in excess of 900 A are reported for layers deposited at 300°C. © 1999 Published by Elsevier Science S.A. All rights reserved.

Simulations of magnetic microstructure in thin film elements used for programmable motion of magnetic particles

The results of two-dimensional micromagnetic modeling of magnetization patterns in Permalloy ellipses under the influence of rotating constant-amplitude magnetic fields are discussed. Ellipses of two different lateral sizes have been studied, 0.5m x 1.5m and 1m x 3m. The amplitude of the rotating magnetic field was varied between simulations with the condition that it must be large enough to saturate or nearly saturate the ellipse with the field applied along the long axis of the ellipse. For the smaller ellipse size it is found that the magnetization pattern forms an S state and the direction of the net magnetization lags behind the direction of the applied field. At a critical angle of the rotating magnetic field the direction of the magnetization switches by a large angle to a new S state. Both the critical angle and the angle interval of the switch depend on field amplitude. For this new state, it is instead the applied field direction that lags behind the magnetization direction. The transient magnetization patterns correspond to multi-domain patterns including two vortices, but this state never exists for the equilibrated magnetization patterns. The behavior of the larger ellipse in rotating field is different. With the field applied along the long-axis of the ellipse, the magnetization of the ellipse is nearly saturated with a vortex close to each apex of the ellipse. As the field is rotated, this magnetization pattern remains and the net-magnetization direction lags behind the direction of the field until for a certain angle of the applied field an equilibrium multi-domain state is created. Comparisons are made with corresponding experimental results obtained by performing in-field magnetic force microscopy on Permalloy ellipses.

Domain configuration of permalloy ellipses in a rotating magnetic field

The domain configuration of micron-sized permalloy ellipses was studied under the influence of an in-plane rotating magnetic field using magnetic force microscopy. The field amplitude was chosen such that when the field is applied parallel to the long axis of the ellipses they are saturated, but when the field is perpendicular to the long axis they exhibit multi-domain states. The rotation angle for nucleation and annihilation of domains was determined for different magnitudes of the applied magnetic field and for two different lateral sizes of ellipses, 6 Am x 2 Am and 3 Am x 1 Am. It was found that both nucleation and annihilation occur over a range of angles for both lateral sizes of ellipses. Saturated states are stable for a wider range of angles for larger values of the applied field.

Micromagnetic studies of Fe/Co ellipses with competing anisotropy contributions

The effects of competing magneto-crystalline and shape anisotropies on magnetization reversal were studied in situ in arrays of sub-micron Fe/Co ellipses of compositions Fe2/Co6 and Fe8/Co3 with magnetic force microscopy (MFM). A simple model assigning magnetization values to the different types of domain structures observed in the MFM images was used to estimate the field dependence of the total magnetization of a sample. The agreement with macroscopic magnetization measurements is discussed. 

Multiferroic domain dynamics in strained strontium titanate

Multiferroicity can be induced in strontium titanate by applying biaxial strain. Using optical second harmonic generation, we report a transition from 4/mmm to the ferroelectric mm2 phase, followed by a transition to a ferroelastic-ferroelectric mm2 phase in a strontium titanate thin film. Piezoelectric force microscopy is used to study ferroelectric domain switching. Second harmonic generation, combined with phase-field modeling, is used to reveal the mechanism of coupled ferroelectric-ferroelastic domain wall motion. These studies have relevance to multiferroics with coupled polar and axial phenomena.

Coexistence of Weak Ferromagnetism and Ferroelectricity in the High Pressure LiNbO_{3}-Type Phase of FeTiO_{3}

We report the magnetic and electrical characteristics of polycrystalline FeTiO3 synthesized at high pressure that is isostructural with acentric LiNbO3 (LBO). Piezoresponse force microscopy, optical second harmonic generation, and magnetometry demonstrate ferroelectricity at and below room temperature and weak ferromagnetism below ~120??K. These results validate symmetry-based criteria and first-principles calculations of the coexistence of ferroelectricity and weak ferromagnetism in a series of transition metal titanates crystallizing in the LBO structure.