SABRINA GONCALVES DE MACEDO CARVALHO

SABRINA GONCALVES DE MACEDO CARVALHO

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W-doped Lanthanum Molybdenum Oxide/Lithium-Sodium-Potassium Carbonate Composite Membranes for Carbon Dioxide Permeation
2023 - MEDINA, MIDILANE S.; CARVALHO, SABRINA G.M.; TABUTI, FRANCISCO N.; MUCCILLO, ELIANA N.S.; FONSECA, FABIO C.; MUCCILLO, REGINALDO
Single-phase tungsten-doped lanthanum molybdenum oxide (La2MoWO9) ceramic powders were synthesized using the complex polymerization technique. Porous ceramic pellets were obtained by thermally removing graphite, which served as a pore former. The porous pellets were then impregnated with molten eutectic lithium-sodium-potassium carbonates. The energy dispersive X-ray analysis and scanning electron microscopy (FEG-SEM) images of the external and fracture surfaces of the La2MoWO9-(Li,Na,K)2CO3 composite dual-phase membrane revealed the percolation of the carbonate mixture through the pores. Electrochemical impedance spectroscopy measurements conducted at temperatures below and above the melting point of the eutectic carbonate composition demonstrated the contributions of oxygen and carbonate ions to the ionic conductivity of the dual membrane. The electrical conductivity of the carbonate ions within the membrane was continuously monitored for over 1300 h with negligible degradation, implying that the membrane could be used for long-term monitoring of CO2 without aging effects. A comparison of FEG-SEM images taken before and after this endurance test suggested minimal fouling, indicating that the membrane could potentially replace similar zirconia- and ceria-based composite membranes.
Design and validation of an experimental setup for evaluation of gas permeation in ceramic membranes
2023 - CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.; MUCCILLO, REGINALDO
An experimental setup for the evaluation of permeation of gaseous species with the possibility of simultaneously collecting electrochemical impedance spectroscopy data in disk-shaped ceramic membranes was designed and assembled. It consists of an alumina sample holder with thermocouple tips and platinum electrodes located close to both sides of the sample. Water-cooled inlet and outlet gas connections allowed for the insertion of the sample chamber into a programmable split tubular furnace. Gas permeation through a ceramic membrane can be monitored with mass flow controllers, a mass spectrometer, and an electrochemical impedance analyzer. For testing and data validation, ceramic composite membranes were prepared with the infiltration of molten eutectic compositions of alkali salts (lithium, sodium, and potassium carbonates) into porous gadolinia-doped ceria. Values of the alkali salt melting points and the permeation rates of carbon dioxide, in agreement with reported data, were successfully collected.
Development of stabilized zirconia–alkali salts dual membranes for carbon dioxide capture
2023 - MUCCILLO, REGINALDO; CARVALHO, SABRINA G.M.; DENALDI, RAFAEL L.; MUCCILLO, ELIANA N.S.
Molten Na2CO3–K2CO3 (NKC, 56–44 mol%) eutectic compositions were vacuum-impregnated, at the eutectic temperature, into two porous ZrO2:8.6 mol% MgO (magnesium-partially stabilized zirconia, MgPSZ) and ZrO2:8 mol% Y2O2 (yttria-fully stabilized zirconia, 8YSZ) ceramics. Thermogravimetric analyses were performed in mixtures of that composition with MgPSZ and 8YSZ ceramic powders. Before impregnation, porosity was achieved in the two compounds by addition and thermal removal of 30 vol.% NKC. To ascertain the carbonates had filled up through the ceramic body, both sides of the parallel and fracture surfaces of the disk-shaped impregnated compositions were observed in a scanning electron microscope and analyzed by energy-dispersive X-ray spectroscopy. The electrical conductivity of the two ceramics, before and after impregnation, was evaluated by electrochemical impedance spectroscopy in the 5 Hz–13 MHz frequency range from approximately 530 to 740°C. The permeation of the carbonate ions through the membranes via the eutectic composition was assessed by the threshold temperatures of the onset of the carbonate ion percolation. The objectives were to prepare dual-phase membranes for the separation of carbon dioxide and for the development of carbon dioxide sensors.
Electric field-assisted sintering anode-supported single solid oxide fuel cell
2022 - MUCCILLO, REGINALDO; FLORIO, DANIEL Z. de; FONSECA, FABIO C.; CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.
Cosintering (La0.84Sr0.16MnO3 thin-film cathode/ZrO2: 8 mol% Y2O3 thin-film solid electrolyte/55 vol.% ZrO2:8 mol% Y2O3 + 45 vol.% NiO anode, ϕ = 12 × 1.5 mm thick pellet) was achieved by applying an electric field for 5 min at 1200°C. Impedance spectroscopy measurements of the anode-supported three-layer cell show an improvement of the electrical conductivity in comparison to that of a conventionally sintered cell. The scanning electron microscopy images of the cross-sections of electric field-assisted pressureless sintered cells show a fairly dense electrolyte and porous anode and cathode. Joule heating, resulting from the electric current due to the application of the AC electric field, is suggested as responsible for sintering. Dilatometric shrinkage curves, electric voltage and current profiles, impedance spectroscopy diagrams, and scanning electron microscopy micrographs show how anode-electrolyte-cathode ceramic cells can be cosintered at temperatures lower than the usually required.
SAXS signature of the lamellar ordering of ionic domains of perfluorinated sulfonic-acid ionomers by electric and magnetic field-assisted casting
2020 - SILVA, JAQUELINE S. da; CARVALHO, SABRINA G.M.; SILVA, RODRIGO P. da; TAVARES, ANA C.; SCHADE, ULRICH; PUSKAR, LJILJANA; FONSECA, FABIO C.; MATOS, BRUNO R.
At present, small angle X-ray scattering (SAXS) studies of perfluorinated sulfonic-acid ionomers (PFSAs) are unable to fully determine the true shape of their building blocks, as recent SAXS modelling predicts disk- and rod-like nanoionic domains as being equally possible. This scenario requires evidence-based findings to unravel the real shape of PFSA building blocks. Herein, a SAXS pattern signature for a lamellar nanophase separation of the ionic domains of Nafion is presented, backed by mid and far infrared spectroscopy (MIR and FIR) and wide angle X-ray scattering (WAXS) data of Nafion in different ionic forms, a broad range of ionic phase contents (EW ~ 859–42 252 g eq-1) and temperatures. The study indicates that the lamellar arrangement of the ionic domains is the most representative morphology that accounts for the physical properties of this ionomer. The lamellar SAXS reflections of Nafion are enhanced in electric and magnetic field-aligned membranes, as confirmed by atomic force microscopy (AFM). Electric and magnetic field-assisted casting of Nafion allowed producing nanostructured and anisotropic films with the lamellas stacked perpendicularly to the field vector, which is the direction of interest for several applications. Such nanostructured Nafion membranes are bestowed with advanced optical and proton transport properties, making them promising materials for solar and fuel cells.
Electric field-assisted pressureless sintering of zirconia–scandia–ceria solid electrolytes
2018 - MUCCILLO, ELIANA N.S.; CARVALHO, SABRINA G.M.; MUCCILLO, REGINALDO
Electric field-assisted (flash) pressureless sintering experiments were carried out in ZrO2 ceramics doped with 10 mol% Sc2O3 and 1 mol% CeO2 (10Sc1CeSZ). All experiments were conducted isothermally at 1050 °C for 2–5 min with the application of a 100–150 V cm−1 AC electric field at 1 kHz with 1–4 A limiting current in green compacts and in samples pre-sintered at different temperatures. Shrinkage level, structural phases and grain morphology data were collected by dilatometry, X-ray diffraction and scanning electron microscopy analyses, respectively. The results showed that for the same delivered electric power, the final shrinkage was higher for higher temperature applications of the electric field and for higher electric current pulses. Moreover, the higher the porosity, the higher the final densification of the flash-sintered 10Sc1CeSZ samples, showing that pores play a role as a preferential path in the flash sintering mechanism.