10 research outputs found

    Preparació d'òxids mesoporosos mitjançant nanocasting

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    S'ha sintetitzat pel mètode de nanocasting pols nanomètrica d'In2O3, NiO i Co3O4 utilitzant diferents mesoestructures de sílice (SBA-16, SBA-15 i KIT-6) com a motlle rígid. Les rèpliques obtingudes s'han caracteritzat amb les tècniques de difracció de raigs X, microscòpia electrònica de rastreig, microscòpia electrònica de transmissió d'alta resolució i BET. L'òxid d'indi, l'òxid de níquel i l'òxid de cobalt obtinguts a partir de la sílice SBA-15 i KIT-6 conserven perfectament l'estructura mesopòrica del motlle, amb valors del diàmetre de porus al voltant dels 7-8 nm. Les rèpliques del motlle SBA-15 estan formades per nanofilaments llargs, mentre que les rèpliques de KIT-6 presenten una estructura hexagonal. A partir del motlle de tipus gàbia (SBA-16), si bé el Co3O4 obtingut és mesopòric, en els altres dos casos (In2O3 i NiO) no s'ha observat ordenament. Per a les rèpliques In2O3 KIT-6 i NiO SBA-15, la caracterització mitjançant BET ha permès corroborar el caràcter mesoestructurat de les mostres.In2O3, NiO and Co3O4 nanopowders were synthesized by the nanocasting method using different silica mesostructures (SBA-16, SBA-15 and KIT-6) as hard templates. The replicas were characterized by X-ray powder diffraction, scanning electron microscopy, high-resolution transmission electron microscopy and BET. The SBA-15 and KIT-6 templated oxides retained the mesoporous structure provided by the template, with pore diameters around 7-8 nm. The SBA-15 replicas were composed of large nanowires, while the KIT-6 replicas displayed a hexagonal structure. On the other hand, though mesoporous Co3O4 powder was achieved by using the cage-like template (SBA-16), no ordering was observed for In2O3 and NiO. For the BET characterization, In2O3 KIT-6 and NiO SBA-15 samples were chosen as a case study, confirming the mesoporous nature of the powders

    Synthesis of compositionally graded nanocast NiO/NiCo2O4/Co3O4 mesoporous composites with tuneable magnetic properties

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    A series of mesoporous NiO/NiCo2O4/Co3O4 composites has been synthesized by nanocasting using SBA-15 silica as a hard template. The evaporation method was used as the impregnation step. Nickel and cobalt nitrates in different Ni(II) : Co(II) molar ratios were dissolved in ethanol and used as precursors. The composites show variable degrees of order, from randomly organized nanorods to highly ordered hexagonally-packed nanowires as the Ni(II) : Co(II) molar ratio decreases. The materials exhibit moderately large surface areas in the 60-80 m2 g−1 range. Their magnetic properties, saturation magnetization (MS) and coercivity (HC), can be easily tuned given the ferrimagnetic (NiCo2O4) and antiferromagnetic (NiO and Co3O4) character of the constituents. Moreover, the NiCo2O4 rich materials are magnetic at room temperature and consequently can be easily manipulated by small magnets. Owing to their appealing combination of properties, the nanocomposites are expected to be attractive for myriad applications

    EEL spectroscopic tomography: Towards a new dimension in nanomaterials analysis

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    Electron tomography is a widely spread technique for recovering the three dimensional (3D) shape of nanostructured materials. Using a spectroscopic signal to achieve a reconstruction adds a fourth chemical dimension to the 3D structure. Up to date, energy filtering of the images in the transmission electron microscope (EFTEM) is the usual spectroscopic method even if most of the information in the spectrum is lost. Unlike EFTEM tomography, the use of electron energy-loss spectroscopy (EELS) spectrum images (SI) for tomographic reconstruction retains all chemical information, and the possibilities of this new approach still remain to be fully exploited. In this article we prove the feasibility of EEL spectroscopic tomography at low voltages (80kV) and short acquisition times from data acquired using an aberration corrected instrument and data treatment by Multivariate Analysis (MVA), applied to FexCo(3-x)O4@Co3O4 mesoporous materials. This approach provides a new scope into materials; the recovery of full EELS signal in 3D

    Controlled 3D-coating of the pores of highly ordered mesoporous antiferromagnetic Co3O4 replicas with ferrimagnetic FexCo3-xO4 nanolayers

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    The controlled filling of the pores of highly ordered mesoporous antiferromagnetic Co3O4 replicas with ferrimagnetic FexCo3-xO4 nanolayers is presented as a proof-of-concept toward the integration of nanosized units in highly ordered, heterostructured 3D architectures. Antiferromagnetic (AFM) Co3O 4 mesostructures are obtained as negative replicas of KIT-6 silica templates, which are subsequently coated with ferrimagnetic (FiM) Fe xCo3-xO4 nanolayers. The tuneable magnetic properties, with a large exchange bias and coercivity, arising from the FiM/AFM interface coupling, confirm the microstructure of this novel two-phase core-shell mesoporous material. The present work demonstrates that ordered functional mesoporous 3D-materials can be successfully infiltrated with other compounds exhibiting additional functionalities yielding highly tuneable, versatile, non-siliceous based nanocomposites

    Preparació d'òxids mesoporosos mitjançant nanocasting

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    S’ha sintetitzat pel mètode de nanocasting pols nanomètrica d’In2O3, NiO i Co3O4 utilitzant diferents mesoestructures de sílice (SBA-16, SBA-15 i KIT-6) com a motlle rígid. Les rèpliques obtingudes s’han caracteritzat amb les tècniques de difracció de raigs X, microscòpia electrònica de rastreig, microscòpia electrònica de transmissió d’alta resolució i BET. L’òxid d’indi, l’òxid de níquel i l’òxid de cobalt obtinguts a partir de la sílice SBA-15 i KIT-6 conserven perfectament l’estructura mesopòrica del motlle, amb valors del diàmetre de porus al voltant dels 7-8 nm. Les rèpliques del motlle SBA-15 estan formades per nanofilaments llargs, mentre que les rèpliques de KIT-6 presenten una estructura hexagonal. A partir del motlle de tipus gàbia (SBA-16), si bé el Co3O4 obtingut és mesopòric, en els altres dos casos (In2O3 i NiO) no s’ha observat ordenament. Per a les rèpliques In2O3 KIT-6 i NiO SBA-15, la caracterització mitjançant BET ha permès corroborar el caràcter mesoestructurat de les mostres.In2O3, NiO and Co3O4 nanopowders were synthesized by the nanocasting method using different silica mesostructures (SBA-16, SBA-15 and KIT-6) as hard templates. The replicas were characterized by X-ray powder diffraction, scanning electron microscopy, high-resolution transmission electron microscopy and BET. The SBA-15 and KIT-6 templated oxides retained the mesoporous structure provided by the template, with pore diameters around 7-8 nm. The SBA-15 replicas were composed of large nanowires, while the KIT-6 replicas displayed a hexagonal structure. On the other hand, though mesoporous Co3O4 powder was achieved by using the cage-like template (SBA-16), no ordering was observed for In2O3 and NiO. For the BET characterization, In2O3 KIT-6 and NiO SBA-15 samples were chosen as a case study, confirming the mesoporous nature of the powders

    Hydrogen sorption performance of MgH2 doped with mesoporous nickel- and cobalt-based oxides

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    The effect of mesoporous Co3O4, NiCo2O4 and NiO on the hydrogen sorption performance of MgH2 was investigated. These oxides were synthesized by multi-step nanocasting and introduced during the high-energy ball milling of MgH2 powder to act as catalysts. Hydrogen desorption on the as-milled powders was assessed upon heating the samples from room temperature to 400°C. In all cases, the onset temperature for desorption was lowered by taking advantage of the introduced additives. The NiO-doped sample displayed the best response, the desorption rate being 7 times faster than in pure MgH2. Complementary kinetic studies on this particular sample revealed that the sorption activation energies were much lower (50 kJ/mol for absorption and 335 kJ/mol for desorption) than the corresponding ones for undoped MgH2 (57 kJ/mol for absorption and 345 kJ/mol for desorption), thus proving the catalytic activity of the mesoporous NiO oxide. Significantly, the X-ray powder diffraction (XRPD) patterns taken on the NiO-doped sample after discharging/charging cycles revealed that Mg could fully hydrogenate at the end of the charging process, while Mg metal was still detected in the undoped (pure) sample. Favored conditions for dissociative chemisorption of hydrogen could be ascribed to the formation of metallic Ni arising from complete or partial reduction of NiO, as observed in the XRPD patterns

    Preparació d'òxids mesoporosos mitjançant nanocasting

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    S'ha sintetitzat pel mètode de nanocasting pols nanomètrica d'In2O3, NiO i Co3O4 utilitzant diferents mesoestructures de sílice (SBA-16, SBA-15 i KIT-6) com a motlle rígid. Les rèpliques obtingudes s'han caracteritzat amb les tècniques de difracció de raigs X, microscòpia electrònica de rastreig, microscòpia electrònica de transmissió d'alta resolució i BET. L'òxid d'indi, l'òxid de níquel i l'òxid de cobalt obtinguts a partir de la sílice SBA-15 i KIT-6 conserven perfectament l'estructura mesopòrica del motlle, amb valors del diàmetre de porus al voltant dels 7-8 nm. Les rèpliques del motlle SBA-15 estan formades per nanofilaments llargs, mentre que les rèpliques de KIT-6 presenten una estructura hexagonal. A partir del motlle de tipus gàbia (SBA-16), si bé el Co3O4 obtingut és mesopòric, en els altres dos casos (In2O3 i NiO) no s'ha observat ordenament. Per a les rèpliques In2O3 KIT-6 i NiO SBA-15, la caracterització mitjançant BET ha permès corroborar el caràcter mesoestructurat de les mostres.In2O3, NiO and Co3O4 nanopowders were synthesized by the nanocasting method using different silica mesostructures (SBA-16, SBA-15 and KIT-6) as hard templates. The replicas were characterized by X-ray powder diffraction, scanning electron microscopy, high-resolution transmission electron microscopy and BET. The SBA-15 and KIT-6 templated oxides retained the mesoporous structure provided by the template, with pore diameters around 7-8 nm. The SBA-15 replicas were composed of large nanowires, while the KIT-6 replicas displayed a hexagonal structure. On the other hand, though mesoporous Co3O4 powder was achieved by using the cage-like template (SBA-16), no ordering was observed for In2O3 and NiO. For the BET characterization, In2O3 KIT-6 and NiO SBA-15 samples were chosen as a case study, confirming the mesoporous nature of the powders

    Erratum to: Guidelines for the use and interpretation of assays for monitoring autophagy (3rd edition) (Autophagy, 12, 1, 1-222, 10.1080/15548627.2015.1100356

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