Associating biosensing properties with the morphological structure of multilayers containing carbon nanotubes on field-effect devices

The control of molecular architecture provided by the layer-by-layer (LbL) technique has led to enhanced biosensors, in which advantageous features of distinct materials can be combined. Full optimization of biosensing performance, however, is only reached if the film morphology is suitable for the principle of detection of a specific biosensor. In this paper, we report a detailed morphology analysis of LbL films made with alternating layers of single-walled carbon nanotubes (SWNTs) and polyamidoamine (PAMAM) dendrimers, which were then covered with a layer of penicillinase (PEN). An optimized performance to detect penicillin G was obtained with 6-bilayer SWNT/PAMAM LbL films deposited on p-Si-SiO(2)-Ta(2)O(5) chips, used in biosensors based on a capacitive electrolyte-insulator-semiconductor (EIS) and a light-addressable potentiometric sensor (LAPS) structure, respectively. Field-emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) images indicated that the LbL films were porous, with a large surface area due to interconnection of SWNT into PAMAM layers. This morphology was instrumental for the adsorption of a larger quantity of PEN, with the resulting LbL film being highly stable. The experiments to detect penicillin were performed with constant-capacitance (Con Cap) and constant-current (CC) measurements for EIS and LAPS sensors, respectively, which revealed an enhanced detection signal and sensitivity of ca. 100 mV/decade for the field-effect sensors modified with the PAMAM/SWNT LbL film. It is concluded that controlling film morphology is essential for an enhanced performance of biosensors, not only in terms of sensitivity but also stability and response time. (C) 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Spectroscopic studies of field-induced electron emission from isolated microstructures

A detailed investigation has been undertaken into the field induced electron emission (FIEE) mechanism that occurs at microscopically localised `sites' on uncoated and dielectric coated metallic electrodes. These processes have been investigated using two dedicated experimental systems that were developed for this study. The first is a novel combined photo/field emission microscope, which employs a UV source to stimulate photo-electrons from the sample surface in order to generate a topographical image. This system utilises an electrostatic lens column to provide identical optical properties under the different operating conditions required for purely topographical and combined photo/field imaging. The system has been demonstrated to have a resolution approaching 1m. Emission images have been obtained from carbon emission sites using this system to reveal that emission may occur from the edge triple junction or from the bulk of the carbon particle. An existing UHV electron spectrometer has been extensively rebuilt to incorporate a computer control and data acquisition system, improved sample handling and manipulation and a specimen heating stage. Details are given of a comprehensive study into the effects of sample heating on the emission process under conditions of both bulk and transient heating. Similar studies were also performed under conditions of both zero and high applied field. These show that the properties of emission sites are strongly temperature and field dependent thus indicating that the emission process is `non-metallic' in nature. The results have been shown to be consistent with an existing hot electron emission model.

Pulsed electric field assisted sol-gel preparation of TiO2 particles and their photocatalytic properties

The objective of this thesis was to study the effect of pulsed electric field on the preparation of TiO2 nanoparticles via sol-gel method. The literature part deals with properties of different TiO2 crystal forms, principles of photocatalysis, sol-gel method and pulsed electric field processing. It was expected that the pulsed electric field would have an influence on crystallite size, specific surface area, polymorphism and photocatalytic activity of produced particles. TiO2 samples were prepared by using different frequencies and treatment times of pulsed electric field. The properties of produced TiO2 particles were examined X-ray diffraction (XRD), Raman spectroscopy and BET surface area analysis. The photocatalytic activities of produced TiO2 particles were determined by using them as photocatalysts for the degradation of formic acid under UVA-light. The photocatalytic activities of samples produced with sol-gel method were also compared with the commercial TiO2 powder Aeroxide® (Evonic Degussa GmbH). Pulsed electric field did not have an effect on the morphology of particles. Results from XRD and Raman analysis showed that all produced TiO2 samples were pure anatase. However, pulsed electric field did have an effect on crystallite size, specific surface area and photocatalytic activity of TiO2 particles. Generally, the crystallite sizes were smaller, specific surface areas larger and initial formic acid degradation rates higher for samples that were produced by applying the pulsed electric field. The higher photocatalytic activities were attributed to larger surface areas and smaller crystallite sizes. Though, with all of the TiO2 samples produced by the sol-gel method the initial formic acid degradation rates were significantly slower than with the commercial TiO2 powder.

Morphology and Blue Photoluminescence Emission of PbMoO(4) Processed in Conventional Hydrothermal

PbMoO(4) micro-octahedrons were prepared by the coprecipitation method at room temperature without the presence of surfactants and processed in a conventional hydrothermal at different temperatures (from 60 to 120 degrees C) for 10 min. These micro-octahedrons were structurally characterized by X-ray diffraction (XRD) and micro-Raman (MR) spectroscopy, and its morphology was investigated by field-emission gun scanning electron microscopy (FEG-SEM). The optical properties were analyzed by ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD patterns and MR spectra confirmed that the PbMoO(4) micro-octahedrons are characterized by a scheelite-type tetragonal structure. FEG-SEM micrographs points, out that these structures present a polydisperse particle size distribution in consequence of a predominant growth mechanism via aggregation of particles. In addition, it was observed that the hydrothermal conditions favored a spontaneous formation of micro-octahedrons interconnected along a common crystallographic orientation (oriented-attachment), resulting in self-organized structures. An intense blue PL emission at room temperature was observed in these micro-octahedrons when they were excited with a 350 nm wavelength. The origin of the PL emissions as well as its intensity variations are explained by means of a model based on both distorted [MoO(4)] and [PbO(8)] clusters into the lattice.

Formation of beta-nickel hydroxide plate-like structures under mild conditions and their optical properties

Nanostructural beta-nickel hydroxide (beta-Ni(OH)(2)) plates were prepared using the microwave hydrothermal (MH) method at a low temperature and short reaction times. An ammonia solution was employed as the coordinating agent, which reacts with [Ni(H(2)O)(6)](2+) to control the growth of beta-Ni(OH)(2) nuclei. A trigonal beta-Ni(OH)(2) single phase was observed by X-ray diffraction (XRD) analyses, and the crystal cell was constructed with structural parameters and atomic coordinates obtained from Rietveld refinement. Field emission scanning electron microscopy (FE-SEM) images revealed that the samples consisted of hexagonal-shaped nanoplates with a different particle size distribution. Broad absorption bands assigned as transitions of Ni(2+) in oxygen octahedral sites were revealed by UV-vis spectra. Photoluminescence (PL) properties observed with a maximum peak centered in the blue-green region were attributed to different defects, which were produced during the nucleation process. We present a growth process scheme of the beta-Ni(OH)(2) nanoplates. (C) 2011 Elsevier Inc. All rights reserved.

Hierarchical Assembly of CaMoO(4) Nano-Octahedrons and Their Photoluminescence Properties

Hierarchical assemblies of CaMoO4 (CM) nano-octahedrons were obtained by microwave-assisted hydrothemial synthesis at 120 degrees C for different times. These structures were structurally, morphologically and optically characterized by X-ray diffraction, micro-Raman spectroscopy, field-emission gun scanning electron microscopy, ultraviolet-visible absorption spectroscopy and photoluminescence measurements. First-principle calculations have been carried out to understand the structural and electronic order-disorder effects as a function of the particle/region size. Supercells of different dimensions were constructed to simulate the geometric distortions along both they and z planes of the scheelite structure. Based on these experimental results and with the help of detailed structural simulations, we were able to model the nature of the order-disorder in this important class of materials and discuss the consequent implications on its physical properties, in particular, the photoluminescence properties of CM nanocrystals.

Morphology and Blue Photoluminescence Emission of PbMoO4 Processed in Conventional Hydrothermal

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Photoluminescence properties and synthesis of a PZT mesostructure obtained by the microwave-assisted hydrothermal method

Micro-cube-shaped lead zirconate titanate was synthesized using the microwave-assisted hydrothermal method. Photoluminescence and field emission scanning electron microscopy were used for monitoring the formation of mesocrystals. Based on these results, a growth mechanism was then proposed which involved nanoparticle aggregation, nanoplate self-assembly on specific architecture and the final formation of mesoscopic micro-cube-shaped lead zirconate titanate. (C) 2011 Elsevier B. V. All rights reserved.

Dielectric properties of Ca(Zr0.05Ti0.95)O-3 thin films prepared by chemical solution deposition

Ca(Zr0.05Ti0.95)O-3 (CZT) thin films were grown on Pt(1 1 1)/Ti/SiO2/Si(1 0 0) substrates by the soft chemical method. The films were deposited from spin-coating technique and annealed at 928 K for 4 h under oxygen atmosphere. CZT films present orthorhombic structure with a crack free and granular microstructure. Atomic force microscopy and field-emission scanning electron microscopy showed that CZT present grains with about 47 nm and thickness about 450 nm. Dielectric constant and dielectric loss of the films was approximately 210 at 100 kHz and 0.032 at 1 MHz. The Au/CZT/Pt capacitor shows a hysteresis loop with remnant polarization of 2.5 mu C/cm(2), and coercive field of 18 kV/cm, at an applied voltage of 6 V. The leakage current density was about 4.6 x 10(-8) A/cm(2) at 3 V. Dielectric constant-voltage curve is located at zero bias field suggesting the absence of internal electric fields. (c) 2006 Elsevier B.V. All rights reserved.

Dependence of annealing time on structural and morphological properties of Ca(Zr0.05Ti0.95)O-3 thin films

Ca(Zr0.05Ti0.95)O-3 (CZT) thin films were prepared by the polymeric precursor method by spin-coating process. The films were deposited on Pt(1 1 1)/Ti/SiO2/Si(1 0 0) substrates and annealed at 650 degrees C for 2,4, and 6 It in oxygen atmosphere. Structure and morphology of the CZT thin films were characterized by the X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM) and field-emission scanning electron microscopy (FEG-SEM). XRD revealed that the film is free of secondary phases and crystallizes in the orthorhombic structure. The annealing time influences the grain size, lattices parameter and in the film thickness. (c) 2006 Elsevier B.V. All rights reserved.

Photolumiscent Properties of Nanorods and Nanoplates Y2O3:Eu3+

Nanorods and nanoplates of Y2O3:Eu3+ powders were synthesized through the thermal decomposition of the Y(OH)(3) precursors using a microwave-hydrothermal method in a very short reaction time. These powders were analyzed by X-ray diffraction, field emission scanning electron microscopy, Fourrier transform Raman, as well as photoluminescence measurements. Based on these results, these materials presented nanoplates and nanorods morphologies. The broad emission band between 300 and 440 nm ascribed to the photoluminescence of Y2O3 matrix shifts as the procedure used in the microwave-hydrothermal assisted method changes in the Y2O3:Eu3+ samples. The presence of Eu3+ and the hydrothermal treatment time are responsible for the band shifts in Y2O3:Eu3+ powders, since in the pure Y2O3 matrix this behavior was not observed. Y2O3:Eu3+ powders also show the characteristic Eu3+ emission lines at 580, 591, 610, 651 and 695 nm, when excited at 393 nm. The most intense band at 610 nm is responsible for the Eu3+ red emission in these materials, and the Eu3+ lifetime for this transition presented a slight increase as the time used in the microwave-hydrothermal assisted method increases.

Very Intense Distinct Blue and Red Photoluminescence Emission in MgTiO3 Thin Films Prepared by the Polymeric Precursor Method: An Experimental and Theoretical Approach

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Microstructural and transport properties of LaNiO3-delta films grown on Si(111) by chemical solution deposition

Electrically conductive LaNiO3-delta (LNO) thin films with typical thickness of 200 nm were deposited on Si (111) substrates by a chemical solution deposition method and heat-treated in air at 700 degreesC. Structural, morphological, and electrical properties of the LNO thin films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), field-emission scanning electron microscopy (FEG-SEM), and electrical resistivity rho(T). The thin films have a very flat surface and no droplet was found on their surfaces. The average grain size observed by AFM and FEG-SEM was approximately 100 nm in excellent agreement with XRD data. The rho(T) data showed that these thin films display a good metallic character in a large range of temperature. These results suggest the use of this conductive layer as electrode in the integration of microelectronic devices. (C) 2003 Elsevier B.V. All rights reserved.

beta-ZnMoO4 microcrystals synthesized by the surfactant-assisted hydrothermal method: Growth process and photoluminescence properties

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

Dielectric properties and microstructure of SrTiO3/BaTiO3 multilayer thin films prepared by a chemical route

Multilayer thin films with perovskite structures were produced by the polymeric precursor method. SrTiO3/BaTiO3 (STO/BTO) multilayers were deposited on Pt(111)/Ti/SiO2/Si(100) substrates by the spin-coating technique and heated in air at 700 degreesC. The microstructure and crystalline phase of the multilayered thin films were examined by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), resolution-high transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and X-ray diffraction. The SrTiO3/BaTiO3 multilayer thin films consisted of grainy structures with an approximate grain size of 60 nm. The multilayered thin films showed a very clear interface between the components. The SrTiO3/BaTiO3 multilayer thin films revealed dielectric constants of approximately 527 and loss tangents of 0.03 at 100 kHz. The dielectric constant calculated for this multilayer film system is the value of the sum of each individual component of the film, i.e. The total value of the sum of each SrTiO3 (STO) and BaTiO3 (BTO) layer. The multilayer SrTiO3/BaTiO3 obtained by the polymeric precursor method, also showed a ferroelectric behavior with a remanent polarization of 2.5 muC/cm(2) and a coercive field of 30 kV/cm. The multilayer films displayed good fatigue characteristics under bipolar stressing after application of 10(10) switching cycles. (C) 2001 Published by Elsevier B.V. B.V. All rights reserved.