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Polymers of intrinsic microporosity exhibit a combination of high gas permeability and reasonable permselectivity, which makes them attractive candidates for gas separation membrane materials. The diffusional selective gas transport properties are connected to the molecular mobility of these polymers in the condensed state. Incoherent quasielastic neutron scattering was carried out on two polymers of intrinsic microporosity, PIM-EA-TB(CH3) and its demethylated counterpart PIM-EA-TB(H2), which have high Brunauer–Emmett–Teller surface area values of 1030 m2 g-1 and 836 m2 g-1, respectively. As these two polymers only differ in the presence of two methyl groups at the ethanoanthracene unit, the effect of methyl group rotation can be investigated solely. To cover a broad dynamic range, neutron time-of-flight was combined with neutron backscattering. The demethylated PIM-EA-TB(H2) exhibits a relaxation process with a weak intensity at short times. As the backbone is rigid and stiff this process was assigned to bendand-flex fluctuations. This process was also observed for the PIM-EA-TB(CH3). A further relaxation process is found for PIM-EA-TB(CH3), which is the methyl group rotation. It was analyzed by a jump-diffusion in a three-fold potential considering also the fact that only a fraction of the present hydrogens in PIM-EATB(CH3) participate in the methyl group rotation. This analysis can quantitatively describe the q dependence of the elastic incoherent structure factor. Furthermore, a relaxation time for the methyl group rotation can be extracted. A high activation energy of 35 kJ mol-1 was deduced. This high activation energy evidences a strong hindrance of the methyl group rotation in the bridged PIM-EA-TB(CH3) structure.
Society is currently confronted with two global challenges, climate change and sustainable development. This reality reverberates amongst the leading nations of the world and is articulated as a priority by the United Nations through the Framework Convention on Climate Change and its seventeen Sustainable Development Goals. In 2016, under the Paris Accord, Mission Innovation, MI, emerged as a global response to climate change and developed eight innovation challenges to mitigate its effect, including Clean Energy Materials, IC6. This innovation challenge focused its efforts on accelerating the development and deployment of clean energy materials by more than a factor of ten through Materials Acceleration Platforms, MAPs – autonomous, self-driving materials laboratories and renewed itself under the current mandate as Materials for Energy, M4E.
Self-driving labs deploy artificial intelligence, robotic automation and high-performance simulation and modeling in a closed loop system of material synthesis and characterization. An international ecosystem for accelerated materials discovery has been established and finds applications in many enabling materials technologies, including nanomaterials. The importance of nanomaterials to catalysis for hydrogen production and carbon dioxide conversion as well as energy storage in batteries is well known. In this work, the international efforts under Materials for Energy will be elaborated including the development of MINERVA - MAP for Intelligent Nanomaterial synthesis Enabled by Robotics for Versatile Applications. MINERVA was specifically built to include the specialized equipment required for the synthesis, characterization and closed-loop optimization of various nano- and advanced materials, ranging from simple inorganic (silica, metal, metal oxide) or polymeric nanoparticles to more complex core-shell architectures and materials with well-defined porosity or surface chemistry. Currently, we are investigating materials for applications in antimicrobial and antibiofouling surface coatings, sensor materials, as well as the reproducible synthesis of reference materials with this platform.
Age-hardenable aluminum alloys undergo precise heat treatments to yield nanometer-sized precipitates that increase their strength and durability by hindering the dislocation mobility. Tensile tests provide mechanical properties, while microstructure evaluation relies on transmission electron microscopy (TEM), specifically the use of dark-field TEM images for precise dimensional analysis of the precipitates. However, this manual process is time consuming, skill dependent, and prone to errors and reproducibility issues.
Our primary goal is to digitally represent these processes while adhering to FAIR principles. Ontologies play a critical role in facilitating semantic annotation of (meta)data and form the basis for advanced data management. Publishing raw data, digital workflows, and ontologies ensures reproducibility.
This work introduces innovative solutions to traditional bottlenecks and offers new perspectives on digitalization challenges in materials science. We support advanced data management by leveraging knowledge graphs and foster collaborative and open data ecosystems that potentially revolutionize materials research and discovery.
The research carried out at the Laboratory of Spectroscopy of Functional Materials at IFSC/USP, in Brazil, is focused on the synthesis and structural-property correlation of luminescent materials including rare-earth (RE) doped glasses, ceramics and hybrid host-guest materials. For the past five years, we have been particularly interested in the development of single- and multifunctional nanosystems based on core-shell upconversion nanoparticles (UCNP) associated with dyes, organometallic complexes and other organic molecules, for biophotonic and sensing applications. In these systems, we take advantage of energy transfer between the UCNPs and the molecules to either supress or enhance luminescent response. Examples include the possibility of bioimaging and photodynamic therapy of bacteria and cancer cells, simultaneous magnetothermia and thermometry, localized O2 sensing, fast detection and quantification of biological markers (e.g. kidney disease) and microorganisms. On what concerns the development of luminescent sensors - a recently started project, our aim is to develop paper-based platforms for point-of-care devices. In this presentation, an overview of our contributions for the past years and our future aims will be presented with several examples.
Recent publications indicate that the order of electrochemical anodization (before or after the laser-processing step) plays an important role for the response of boneforming osteoblasts – an effect that can be utilized for improving permanent dental- or removable bone-implants. For exploring these different surface functionalities, multi-method chemical and structural characterizations were performed for two different characteristic micro-spikes covered by nanometric laserinduced periodic surface structures (LIPSS) on Ti-6Al-4V upon irradiation with nearinfrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 66 & 80 kHz pulse repetition rate) at two distinct sets of laser fluence and beam scanning parameters. This involves morphological and topographical investigations by scanning electron microscopy (SEM) and white light interference microscopy (WLIM), near-surface chemical analysis by X-ray photoelectron spectroscopy (XPS) and hard X-ray photoelectron spectroscopy (HAXPES), as well as structural material examination via X-ray diffraction (XRD) measurements. The results allow to qualify the laser ablation depth, assess the spike geometry and surface roughness parameters, and provide detailed insights into the near-surface oxidation that may cause the different cell growth behavior for pre- or post-anodized medical implants.
Quantum dots (QDs) are remarkable semiconductor nanoparticles, whose optical properties are strongly size-dependent. Therefore, the real-time monitoring of crystal growth pathway during synthesis gives an excellent opportunity to a smart design of the QDs luminescence. In this work, we present a new approach for monitoring the formation of QDs in aqueous solution up to 90 °C, through in situ luminescence analysis, using CdTe as a model system. This technique allows a detailed examination of the evolution of their light emission. In contrast to in situ absorbance analysis, the in situ luminescence measurements in reflection geometry are particularly advantageous once they are not hindered by the concentration increase of the colloidal suspension. The synthesized particles were additionally characterized using X-ray diffraction analysis, transition electron microscopy, UV-Vis absorption and infrared spectroscopy. The infrared spectra showed that 3-mercaptopropionic acid (MPA)-based thiols are covalently bound on the surface of QDs and microscopy revealed the formation of CdS. Setting a total of 3 h of reaction time, for instance, the QDs synthesized at 70, 80 and 90 °C exhibit emission maxima centered at 550, 600 and 655 nm. The in situ monitoring approach opens doors for a more precise achievement of the desired emission wavelength of QDs.
Upconverting nanoparticles are essential in modern photonics due to their ability to convert infrared light to visible light. Despite their significance, they exhibit limited brightness, a key drawback that can be addressed by combining them with plasmonic nanoparticles. Plasmon-enhanced upconversion has been widely demonstrated in dry environments, where upconverting nanoparticles are immobilized, but constitutes a challenge in liquid media where Brownian motion competes against immobilization.
This study employs optical tweezers for the three-dimensional manipulation of an individual upconverting nanoparticle, enabling the exploration of plasmon-enhanced upconversion luminescence in water. Contrary to expectation, experiments reveal a long-range (micrometer scale) and moderate (20%) enhancement in upconversion luminescence due to the plasmonic resonances of gold nanostructures. Comparison between experiments and numerical simulations evidences the key role of Brownian motion. It is demonstrated how the three-dimensional Brownian fluctuations of the upconverting nanoparticle lead to an “average effect” that explains the magnitude and spatial extension of luminescence enhancement.
Surface-modification platforms that are universally applicable are vital for the development of new materials, surfaces, and nanoparticles. Mussel-inspired materials (MIMs) are widely used in various fields because of their strong adhesive properties and post-functionalization reactivity. However, conventional MIM coating techniques have limited deposition selectivity and lack structural control, which has limited their use in microdevices that require full control over deposition. To overcome these limitations, we developed a micropatterning technique for MIMs using multiphoton lithography, which does not require photomasks, stamps, or multistep procedures. This method enables the creation of MIM patterns with micrometer resolution and full design freedom and paves the way for innovative applications of MIMs in various multifunctional systems and microdevices, such as microsensors, MEMS, and microfluidics.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge with CS technology is that most of the process technology has to be developed anew to the high standards required by electronic applications. Today, compound semiconductors can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). With this method, many different compounds with semiconducting properties can be synthesized. Additionally, this process technology is a direct thin layer deposition method. Therefore, complex multilayer systems can be generated directly by the deposition process and without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process of these thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and number density, as well as to characterise defects for process optimisation.
We report here on the use of spectroscopic ellipsometry and imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN materials as well as oxidised SiC surfaces. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is called imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry method like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge is that most of the process technology has to be developed specifically and tailored to the high standards required by electronic applications. Today, many different CS materials can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). This technology is a direct thin layer deposition method capable of producing complex multilayer systems directly from one deposition process without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process when targeting electronic thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and density, as well as to characterise defects for further process optimisation.
We report here on the use of spectroscopic and multispectral imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN as well as oxidised SiC. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is known as imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry methods like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.