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Projeto de investigação
3D printed TiO2 photocatalysts for green urea production, water purification and CO2 capture under sunlight
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Microwave Synthesis of Visible-Light-Activated g-C3N4/TiO2 Photocatalysts
Publication . Matias, Maria Leonor; Reis-Machado, Ana S.; Rodrigues, Joana; Calmeiro, Tomás; Deuermeier, Jonas; Pimentel, Ana; Fortunato, Elvira; Martins, Rodrigo; Nunes, Daniela; UNINOVA-Instituto de Desenvolvimento de Novas Tecnologias; CENIMAT-i3N - Centro de Investigação de Materiais (Lab. Associado I3N); DCM - Departamento de Ciência dos Materiais; LAQV@REQUIMTE; DQ - Departamento de Química; MDPI AG
The preparation of visible-light-driven photocatalysts has become highly appealing for environmental remediation through simple, fast and green chemical methods. The current study reports the synthesis and characterization of graphitic carbon nitride/titanium dioxide (g-C3N4/TiO2) heterostructures through a fast (1 h) and simple microwave-assisted approach. Different g-C3N4 amounts mixed with TiO2 (15, 30 and 45 wt. %) were investigated for the photocatalytic degradation of a recalcitrant azo dye (methyl orange (MO)) under solar simulating light. X-ray diffraction (XRD) revealed the anatase TiO2 phase for the pure material and all heterostructures produced. Scanning electron microscopy (SEM) showed that by increasing the amount of g-C3N4 in the synthesis, large TiO2 aggregates composed of irregularly shaped particles were disintegrated and resulted in smaller ones, composing a film that covered the g-C3N4 nanosheets. Scanning transmission electron microscopy (STEM) analyses confirmed the existence of an effective interface between a g-C3N4 nanosheet and a TiO2 nanocrystal. X-ray photoelectron spectroscopy (XPS) evidenced no chemical alterations to both g-C3N4 and TiO2 at the heterostructure. The visible-light absorption shift was indicated by the red shift in the absorption onset through the ultraviolet-visible (UV-VIS) absorption spectra. The 30 wt. % of g-C3N4/TiO2 heterostructure showed the best photocatalytic performance, with a MO dye degradation of 85% in 4 h, corresponding to an enhanced efficiency of almost 2 and 10 times greater than that of pure TiO2 and g-C3N4 nanosheets, respectively. Superoxide radical species were found to be the most active radical species in the MO photodegradation process. The creation of a type-II heterostructure is highly suggested due to the negligible participation of hydroxyl radical species in the photodegradation process. The superior photocatalytic activity was attributed to the synergy of g-C3N4 and TiO2 materials.
Floating TiO2-Cork Nano-Photocatalysts for Water Purification Using Sunlight
Publication . Matias, Maria Leonor; Morais, Maria; Pimentel, Ana; Vasconcelos, Francisco X.; Reis Machado, Ana S.; Rodrigues, Joana; Fortunato, Elvira; Martins, Rodrigo; Nunes, Daniela; UNINOVA-Instituto de Desenvolvimento de Novas Tecnologias; CENIMAT-i3N - Centro de Investigação de Materiais (Lab. Associado I3N); DCM - Departamento de Ciência dos Materiais; LAQV@REQUIMTE; DQ - Departamento de Química; Molecular Diversity Preservation International (MDPI)
In the present study, titanium dioxide (TiO2) nano-photocatalysts were synthesized through microwave irradiation. In a typical microwave synthesis, TiO2 nanomaterials were simultaneously produced in powder form and also directly covering cork substrates. The TiO2 nanopowder was analyzed by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM), revealing that the solvothermal microwave synthesis resulted only in the TiO2 anatase phase. From Fourier-transform infrared spectroscopy (FTIR), cork’s organic species, along with bands of TiO2, were detected. UV–VIS absorption spectrum revealed an absorption extension to the visible region, since a brown powdered TiO2 product was obtained. Very fine nanoparticles were observed displaying a nearly spherical shape that agglomerates in larger particles. These larger particles fully covered the surface of the honeycomb cork cells, originating TiO2 functionalized cork platforms. The TiO2 functionalized substrates were further tested as floating photocatalysts and their photocatalytic activity was assessed from rhodamine B degradation under solar simulating light and natural sunlight. Reusability tests were also performed under natural sunlight. The strategy applied in this research work allowed the production of green and low-cost cork platforms based on TiO2 photoactive materials with the ability to purify polluted water under natural sunlight.
A Comparison between Solution-Based Synthesis Methods of ZrO2 Nanomaterials for Energy Storage Applications
Publication . Matias, Maria Leonor; Carlos, Emanuel; Branquinho, Rita; do Valle, Hadassa; Marcelino, João; Morais, Maria; Pimentel, Ana; Rodrigues, Joana; Monteiro, Teresa; Fortunato, Elvira; Martins, Rodrigo; Nunes, Daniela; UNINOVA-Instituto de Desenvolvimento de Novas Tecnologias; CENIMAT-i3N - Centro de Investigação de Materiais (Lab. Associado I3N); DCM - Departamento de Ciência dos Materiais; MDPI - Multidisciplinary Digital Publishing Institute
The present study is focused on the synthesis of zirconium dioxide (ZrO2) nanomaterials using the hydrothermal method assisted by microwave irradiation and solution combustion synthesis. Both synthesis techniques resulted in ZrO2 powders with a mixture of tetragonal and monoclinic phases. For microwave synthesis, a further calcination treatment at 800 °C for 15 min was carried out to produce nanopowders with a dominant monoclinic ZrO2 phase, as attested by X-ray diffraction (XRD) and Raman spectroscopy. The thermal behavior of the ZrO2 nanopowder was investigated by in situ XRD measurements. From the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images, the presence of near spherical nanoparticles was clear, and TEM confirmed the ZrO2 phases that comprised the calcinated nanopowders, which include a residual tetragonal phase. The optical properties of these ZrO2 nanopowders were assessed through photoluminescence (PL) and PL excitation (PLE) at room temperature (RT), revealing the presence of a broad emission band peaked in the visible spectral region, which suffers a redshift in its peak position, as well as intensity enhancement, after the calcination treatment. The powder resultant from the solution combustion synthesis was composed of plate-like structures with a micrometer size; however, ZrO2 nanoparticles with different shapes were also observed. Thin films were also produced by solution combustion synthesis and deposited on silicon substrates to produce energy storage devices, i.e., ZrO2 capacitors. The capacitors that were prepared from a 0.2 M zirconium nitrate-based precursor solution in 2-methoxyethanol and annealed at 350 °C exhibited an average dielectric constant (κ) of 11 ± 0.5 and low leakage current density of 3.9 ± 1.1 × 10−7 A/cm2 at 1 MV/cm. This study demonstrates the simple and cost-effective aspects of both synthesis routes to produce ZrO2 nanomaterials that can be applied to energy storage devices, such as capacitors.
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Entidade financiadora
Fundação para a Ciência e a Tecnologia
Programa de financiamento
OE
Número da atribuição
UI/BD/151292/2021