55 research outputs found

    Scale up of microwave annealed FA0.83Cs0.17PbI1.8Br1.2 perovskite towards an industrial scale

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    ABSTRACT: Perovskite solar cells (PSCs) efficiency has rapidly increased from the initial 3.8 to recent 24.2%. This high efficiency has attracted serious worldwide researchers and industry attention due to their low material cost, and simple solution-based fabrication process. However, fundamental studies on PSCs are usually produced through lab-scale actions and carried out on small-area devices (≤1 cm2). Here we present the advances of up-scaling using microwave (MW) annealing of perovskite films on large area specimens (~16 cm2), looking forward the industrial-scale. Morphological, structural and optical characterization were performed to confirm the effectiveness of the scaled up MW annealing.info:eu-repo/semantics/publishedVersio

    Looking into historical cracks analysing repaired silver objects by electron microscopy

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    ABSTRACT: The identification of structural alterations of silver alloy objects of cultural interest is essential to assess their state of conservation and define maintenance programmes. Alterations induced by previous repair and cleaning actions strongly affect the conservation condition, influencing the type and extension of conservation procedures. The detailed analysis of ancient repairs is a subject to be investigated. In this work, we show the potentialities of scanning electron microscopy in the characterisation of structural repairs and their influence on the conservation state of silver objects. The study of distinct silver objects dated to the 16th and 18th centuries allowed us to show, among others, the non-intentional dealloying of copper due to the use of acid solutions in surface cleanings and cracks resulting from incorrect handling. The data collected by microscopic examination contributed to the definition of preservation and maintenance methodologies applied to those silver objects.info:eu-repo/semantics/publishedVersio

    Diagnosis of pathologies in ancient (seventeenth-eighteenth centuries) decorative blue-and-white ceramic tiles : Green stains in the glazes of a panel depicting Lisbon prior to the 1755 earthquake

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    Decorative panels of ceramic glazed tiles comprise a valuable cultural heritage in Mediterranean countries. Their preservation requires the development of a systematic scientific approach. Exposure to an open-air environment allows for a large span of deterioration effects. Successfully overcoming these effects demands a careful identification of involved degradation processes. Among these, the development of micro-organisms and concomitant glaze surface staining is a very common effect observed in panels manufactured centuries ago. This paper describes a study on the nature of green stains appearing at the surface of blue-and-white tile glazes from a large decorative panel with more than one thousand tiles, called Vista de Lisboa that depicts the city before the destruction caused by the 1755 earthquake. The characterization of green-stained blue-and-white tile glazes was performed using non-destructive X-ray techniques (diffraction and fluorescence spectrometry) by directly irradiating the surface of small tile fragments, complemented by a destructive scanning electron microscopy (SEM) observation of one fragment. Despite the green staining, analytical X-ray data showed that no deterioration had occurred irrespective of the blue or white color, while complementary SEM-EDX data provided chemical evidence of microorganism colonization at the stained glaze surface

    Environmental status of water and sediment around submarine outfalls – west coast of Portugal = Qualidade da água e dos sedimentos na zona circundante de oito emissários submarinos – costa oeste de Portugal

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    The sea along the western coast of Portugal presents hydrodynamic conditions that place it among the most favourable of European coastal waters for dilution and dispersion of waste water. Thus it is an appropriate zone for the location of submarine outfalls. According to the European Union Directives and Portuguese Regulations the waste waters produced by this densely populated coast should be treated, therefore 18 wastewater treatment plants with submarine outfalls were built along the coast. Between 2002 and 2004, five sampling campaigns were performed in seven outfalls that were selected to participate in water and sediment quality surveys supported by INAG (Portuguese Water Institute), and performed by the Hydrographic Institute of the Portuguese Navy. The water quality assessment was based on 10 chemical and physical parameters, including heavy metals. The results were compared with reference values and data from the largest flow outfall located at Guia, which has an autonomous monitoring program. In order to evaluate significant differences in water quality between years and sampling sites, statistical analyses were performed. S ediments were evaluated for grain size, heavy metals, PAH, hydrocarbons, chlorinated pesticides and PCB. In order to evaluate the level of pollution of the different areas where the outfalls are located, the concentration factor (CF) (sediment/water elemental concentration ratio) was calculated and compared with the recommended values for the CF of each element. The water sampling program did not allow identifying a clear seasonal evolutionary pattern. The environmental status of the waters surrounding the outfalls discharges comply, to a great extent, with the reference values proposed by INAG and did not revel high levels of contaminants. Due to the low sorptive capacity of the sediment for contaminants, trace metals, hydrocarbons and PAHs have a low environmental impact. The values of the concentration factors for metals are below the recommended values

    When gold stops glittering: corrosion mechanisms of René Lalique's Art Nouveau jewellery

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    ABSTRACT: Art Nouveau jewellery created by René Lalique is presently corroded. To identify the corrosion processes, Au-Ag-Cu alloys with compositions comparable to those used in the René Lalique’s jewellery were fabricated to be exposed to sulphide-containing environments. Using SEM-EDS, XRD, UV-Vis spectroscopy and ellipsometry, it was for the first time demon-strated that at the surface of tarnished Au alloys forms a corrosion film with a layer-by-layer structure. Considering the complex refractive indices of bulk Cu and Ag oxides and sulphides, a two-step corrosion mechanism was proposed. The formation of Cu-based compounds during the early corrosion stages is followed by the formation of Ag-based compounds. The thinness of the formed film, shown for one of the gold alloys to be of 80 nm, is due to a corrosion kinetics controlled by the presence of Au and by the formation of an Au-S self-assembled monolayer. The corrosion mechanism of gold alloys raises a new conservation challenge concerning the removal of nanometric layers.info:eu-repo/semantics/publishedVersio

    Charge transport and recombination of dye sensitized 1D nanostructured-TiO2 films prepared by reactive sputtering

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    Dye sensitized solar cells (DSCs) are governed by light absorption, charge injection, electron transport and recombination and electrolyte diffusion. One way to improve the efficiency of these devices is by the design of highly ordered nanostructured semiconductor materials.The advantages can be two-fold: Firstly charge transport within the metal-oxide can be enhanced and hence thicker films can be employed and secondly, the complete permeation with a solid-state hole-transport medium of the sensitized metal-oxide can be facilitated. Nanostructured materials should promote vectorial electron diffusion and have as few recombination sights as possible so as to further enhance electron lifetimes and electron collection efficiencies. These materials should also have a high surface area so as to allow for efficient dye-loading and hence light absorption. Highly ordered TiO2 nanostructured films were prepared by reactive sputtering and their charge transport characteristics evaluated in DSCs. These were compared to DSCs employing mesoporous TiO2 films prepared by doctor blade technique using commercial paste. Charge transport characteristics were evaluated by impedance spectroscopy (IS), incident photon to current conversion efficiencies (IPCE) and current-voltage (iV) curves under simulated AM1.5G irradiation. Film morphology and structural properties were evaluated by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively

    Assessment of dye distribution in sensitized solar cells by microprobe techniques

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    Dye sensitized solar cells (DSCs) have received considerable attention once this technology offers economic and environmental advantages over conventional photovoltaic (PV) devices. The PV performance of a DSC relies on the characteristics of its photoanode, which typically consists of a nanocrystalline porous TiO2 film, enabled with a large adsorptive surface area. Dye molecules that capture photons from light during device operation are attached to the film nanoparticles. The effective loading of the dye in the TiO2 electrode is of paramount relevance for controlling and optimizing solar cell parameters. Relatively few methods are known today for quantitative evaluation of the total dye adsorbed on the film. In this context, microprobe techniques come out as suitable tools to evaluate the dye surface distribution and depth profile in sensitized films. Electron Probe Microanalysis (EPMA) and Ion Beam Analytical (IBA) techniques using a micro-ion beam were used to quantify and to study the distribution of the Ru organometallic dye in TiO2 films, making use of the different penetration depth and beam sizes of each technique. Different 1D nanostructured TiO2 films were prepared, morphologically characterized by SEM, sensitized and analyzed by the referred techniques. Dye load evaluation in different TiO2 films by three different techniques (PIXE, RBS and EPMA/WDS) provided similar results of Ru/Ti mass fraction ratio. Moreover, it was possible to assess dye surface distribution and its depth profile, by means of Ru signal, and to visualize the dye distribution in sample cross-section through X-ray mapping by EPMA/EDS. PIXE maps of Ru and Ti indicated an homogeneous surface distribution. The assessment of Ru depth profile by RBS showed that some films have homogeneous Ru depth distribution while others present different Ru concentration in the top layer (2 lm thickness). These results are consistent with the EPMA/EDS maps obtained

    Microscopy techniques for dye distribution in DSCs nanocrystalline TiO2 films 

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    Capture of sunlight has attracted an increasing interest in the scientific community and triggered the development of efficient and cheap photovoltaic devices. Amongst recent generation technologies for solar energy conversion, dye-sensitized solar cells (DSCs) show an optimal trade-off between high-conversion efficiency and low-cost manufacturing. For the last two decades, significant progress has been made and best energy conversion efficiency of the DSC at the laboratory scale has surpassed 12% [1]. A lot of work has focused on the enlargement of surface areas to enhance the amount of adsorbed dyes by reduction of nanoparticle sizes or utilization of novel structures. Nevertheless there remain some crucial details of DSC operation for which limited information is available, namely dye diffusion and adsorption, surface coverage and dye distribution throughout the nc-TiO2 film. Microprobe techniques can be powerful tools to evaluate the dye load, the dye distribution and dye depth profile in sensitized films. Electron Probe Microanalysis (EPMA) and Ion Beam Analytical (IBA) techniques using a micro-ion beam, namely micro-Particle Induced X-ray Emission ( PIXE) and Rutherford Backscattering Spectrometry (RBS), were used to quantify and to study the distribution of the ruthenium organometallic (N719) dye in TiO2 films, profiting from the different penetration depth and beam sizes of each technique. Two different types of films were prepared and sensitized, mesoporous nanoparticles and 1D nanostructured TiO2 films (figure 1). Despite the low concentration of Ru, the high sensitive analytical techniques used allowed to assess the Ru surface distribution and depth profile. Fig. 2 shows the PIXE maps of Ru and Ti indicating an homogeneous surface distribution. The same figure presents the RBS spectra obtained with a 2 MeV proton beam of the same sample showing that a good spectra fit is obtained considering only two sample layers: the first one with a 1.7 ìm thickness; the second one being the SiO2 substrate. The Ru RBS signal also shows that the dye has an homogeneous depth distribution. Due to the fine spatial resolution of the EPMA/WDS (Wavelength Dispersive Spectroscopy) technique it was possible to visualise the dye distribution in sample cross-section (with micrometer or submicrometer dimensions) as presented in Fig. 3 for the elemental mapping of a mesoporous nanoparticle TiO2 film. Dye load evaluation by two different techniques (ìPIXE and EPMA/WDS) provided similar results (Ru/Ti values around 0.5 %). The distribution analysis of the organometallic dye (N719) was done through ruthenium distribution via X-ray mapping. RBS was used to assess the ruthenium depth profile. This assessment can lead to a better understanding of the device performance
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