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.
Tape-casting and freeze-drying gadolinia-doped ceria composite membranes for carbon dioxide permeation
2022 - CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.; FONSECA, FABIO C.; MULLER, MICHAEL; SCHULZE-KUPPERS, FALK; BAUMANN, STEFAN; MEULENBERG, WILHELM A.; GUILLON, OLIVIER; MUCCILLO, REGINALDO
Porous ceria: 20 mol% gadolinia (20GDC) ceramic membranes were prepared by tape casting (TC) and freeze-drying (FD) techniques, obtaining ceramic matrices with randomly dispersed round pores and with an aligned pore structure, respectively. Samples were sintered at 1450 °C, followed by infiltration of molten eutectic sodium-lithium carbonates (NLC). The pore morphology of 20GDC-TC and 20GDC-FD composite membranes was evaluated by analysis of scanning electron microscopy images. The electrical resistivity was determined by electrochemical impedance spectroscopy in the 1 Hz - 10 MHz frequency range from 300 °C to 700 °C, covering the solid-to-molten NLC temperature range, showing that the aligned pore structure improved the conductivity of the ceramic matrix in addition to facilitating molten carbonate infiltration, improving the total (bulk + interfaces) electrical conductivity of the composite membrane. Permeation experiments showed high CO2 permeation rates reached 5.35 × 10−7 mol m−2 s−1 Pa−1 at 800 °C. The infiltration of molten sodium-lithium carbonate in gadolinium-doped ceria prepared by the freeze-drying technique is proposed as an optimized procedure for producing membranes for carbon dioxide separation.
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 sintering (gadolinia-doped ceria/alkali salts) composite membranes
2020 - CARVALHO, S.G.M.; MUCCILLO, E.N.S.; MARQUES, F.M.B.; MUCCILLO, R.
Composite ceramic membranes were prepared according to two routes: (i) vacuum impregnation of molten eutec- tic sodium-lithium carbonates (NLC) into porous ceria-20 mol% gadolinia (20GDC) solid electrolytes; (ii) electric field-assisted sintering of a 25 wt% NLC/75 wt% 20GDC mixture. Porous 20GDC ceramics were obtained by controlled thermal removal of 40 vol% KCl added as pore former. Electric field-assisted (flash) sintering was car- ried out monitoring thickness during application of 200 V cm − 1 to the specimen positioned in a sample chamber inserted in a vertical dilatometer. The surfaces of the sintered membranes were observed in a scanning electron microscope. Electrochemical impedance spectroscopy measurements were performed in the 5 Hz to 13 MHz fre- quency range in the 280–580°C range. Arrhenius plots showed the transition from oxide ion conduction (due to the solid electrolyte) to carbonate ion conduction (due to the molten NLC). Membranes flash sintered at 420°C in 2 min showed electrical conductivity similar to membranes conventionally sintered at 690°C for 2 h.
Enhancement of the ionic conductivity in electric field-assisted pressureless sintered BITIVOX solid electrolytes
2019 - MEDINA, MIDILANE S.; CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.; MUCCILLO, REGINALDO
Bi4V1.8Ti0.2O11 (BITIVOX) ceramic pellets, prepared with powders obtained by a sol gel technique, were sintered either conventionally at 800 C/8 h or by applying an AC electric voltage, limiting the electric current through the pellets. Electric voltages were applied isothermally at 700 C and 800 C during 5 min in the green pellet positioned in the sample holder of a dilatometer for monitoring thickness variation. The BITIVOX pellets shrank 13.6% after applying 200 V cm􀀀1 at 800 C and 10.4% heating to 800 C for 8 h. Thermal analysis and X-ray di raction of the powders were performed to evaluate the crystallization temperature and the structural phase, respectively. The electrical behavior of the sintered BITIVOX pellets was analyzed by the impedance spectroscopy technique, showing that the sample flash sintered at 800 C/5 min had lower bulk resistivity than the sample conventionally sintered at 800 C/8 h. The surfaces of the sintered pellets were observed in a scanning electron microscope showing similar grain sizes and pore content in all sintered samples.
Electrical behavior of electric field-assisted pressureless sintered ceria-20 mol% samaria
2019 - REIS, SHIRLEY L.; CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.; MUCCILLO, REGINALDO
CeO2:20 mol% Sm2O3 green ceramic pellets were sintered conventionally at 1500 C/2 h and flash sintered by applying a 200 V cm􀀀1 electric field at 800 C, 1000 C and 1200 C. The thickness shrinkage of the pellets was followed bythe specimen being positioned inside a dilatometer adapted with platinum electrodes and terminal leads connected to a power supply for application of the electric voltage. The microstructure of the surfaces of the sintered samples were observed in a scanning electron microscope. The electrical properties were evaluated by the impedance spectroscopy technique in the 5 Hz–13 MHz frequency range from 210 C to 280 C. The main results show that (i) the final shrinkage level is nearly independent of the temperature when the electric field is applied and slightly better than that of the 1500 C sintered pellet, and (ii) the bulk conductivity of the sample flash sintered at 1200 C is similar to that of the sample sintered at 1500 C. The availability of a pathway for the electric current pulse derived from the applied electric field is proposed as the reason for the achieved shrinkages. Scavenging of the grain boundaries by Joule heating is proposed as the reason for the improved oxide ion bulk conductivity.
Electrical behavior and microstructural features of electric field-assisted and conventionally sintered 3 mol % yttria-stabilized zirconia
2018 - CARVALHO, SABRINA G.M.; MUCCILLO, ELIANA N.S.; MUCCILLO, REGINALDO
ZrO2: 3 mol % Y2O3 (3YSZ) polycrystalline pellets were sintered at 1400 C and by applying an alternating current (AC) electric field at 1000 C. An alumina sample holder with platinum wires for connecting the sample to a power supply was designed for the electric field-assisted sintering experiments. The apparent density was evaluated with the Archimedes technique, the grain size distribution by analysis of scanning electron microscopy images, and the electrical behavior by the impedance spectroscopy technique. Sintering with the application of AC electric fields to 3YSZ enhances its ionic conductivity. An explanation is proposed, based on the dissolution back to the bulk of chemical species, which are depleted at the grain boundaries, leading to an increase in the oxygen vacancy concentration. For the enhancement of the grain boundary conductivity, an explanation is given based on the diminution of the concentration of depleted chemical species, which migrate to the bulk. This migration leads to a decrease of the potential barrier of the space charge region, known to be responsible for blocking the oxide ions through the intergranular region. Moreover, the heterogeneity of the distribution of the grain sizes is ascribed to the skin effect, the tendency of the AC current density to be largest near the surface, decreasing towards the bulk.