Nanocomposites hold great promise for enhancing material properties beyond those of conventional materials. Here, we present a novel method integrating template-assisted electrodeposition of nanocrystalline gold (nc Au) and atomic layer deposition (ALD) of alumina to fabricate three-dimensional nanostructured metal matrix composites (MMCs) with enhanced mechanical strength, reduced density, and improved thermal stability. Microcompression experiments demonstrate that Au-alumina MMC achieves a yield strength of 838 MPa, outperforming pure nc Au (792 MPa) and Au hollow microlattices (250 MPa). The strength advantage increases at elevated temperatures: the MMC exhibits a 5 % improvement in yield strength at room temperature while retaining only 80 % of the weight, rising to a 42 % improvement at 100 degrees C. To enable design and optimization of such nanocomposites, we performed a systematic thermomechanical study on pure nc Au. Compression tests across a range of temperatures (23 degrees C to 100 degrees C) and strain rates (0.0004 s-1 to 216 s-1) revealed a transition in deformation behavior around 1 s-1 . In the quasistatic regime, strain rate sensitivity increased from 0.025 to 0.063 with temperature, while remaining low (0.013) and temperature-independent at higher strain rates. The increase in activation volume (10 b3 to 24 b3) and activation energy (49-83 kJ/mol) with strain rate suggests a change in the rate-controlling mechanism. These results provide essential input for finite element modeling (FEM) of MMC, enabling identification of architectural parameters that can be tuned to optimize strength before fabrication. This work demonstrates the potential of microscale additive manufacturing and hybrid fabrication strategies to produce nanocomposites with tunable thermomechanical properties for demanding structural applications.
Expanding fluorescence bioimaging into the second near-infrared spectrum (NIR-II, 1000-1700 nm) unlocks advanced possibilities for diagnostics and therapeutics, offering superior tissue penetration and resolution. Two-dimensional copper tetrasilicate (CTS) pigments (MCuSi4O10, M = Ca, Sr, Ba) are known for their brightness and stability, yet synthetic challenges have curbed their integration into bioimaging. Here, we introduce flame-spray-pyrolysis (FSP) as a versatile and scalable synthesis approach to produce ultra-bright, metastable CTS nanosheets (NS) by annealing multi-element metal oxide nanoparticles into 2D crystals. Group-II ion incorporation shifts emission into the NIR-II range, with Ba0.33Sr0.33Ca0.33CuSi4O10 peaking at 1007 nm, while minor Mg-doping induces a hypsochromic shift and extends fluorescence lifetimes. The engineered CTS achieve quantum yields up to 34%, supporting NS high-frame-rate imaging (>200 fps). These unique properties enable CTS-NS to serve as powerful contrast agents for super-resolution NIR bioimaging, demonstrated in vivo through transcranial microcirculation mapping and macrophage tracking in mice using diffuse optical localization imaging (DOLI). This pioneering synthesis strategy unlocks wavelength-tunable NS for advanced NIR-II bioimaging applications.
Abstract A series of 54 experiment cycles were performed on an FeCr21Ni19 (at. %) sample in vacuum, He and Ar gas atmospheres using the Electromagnetic Levitation facility onboard the International Space Station (ISS-EML). Evaporation control is a critical facility resource that limits processing time and must be tracked to ensure astronaut safety. Species specific evaporation during this test has been estimated using a mathematical model based on thermodynamic assessment and Langmuir’s equation to track the dynamic mass loss during each thermal cycle. The findings from this study were validated using post-mission SEM-EDX evaluations. The predicted mass loss and elemental distribution from the evaporation model was consistent with experimental observations. Based on facility geometry, deposit layer thicknesses at various locations have also been calculated and results showed excellent agreement with near-real-time predictions using software developed by the German Space Agency (DLR) Microgravity User Support Center (MUSC).
Evaporation control is a critical facility resource during solidification experiments that limits processing time and must be tracked to ensure facility health. A thermodynamic analysis was performed on a ternary FeCrNi sample processed onboard the International Space Station (ISS) using ESA Electromagnetic Levitation (EML) facility in a microgravity environment. A non-ideal solution-based mathematical model was applied for the overall sample mass loss prediction during this study. The overall sample mass loss prediction is consistent with the post-flight mass loss measurements. The species-specific findings from this study were validated using post-mission SEM-EDX surface evaluations by three different facilities. The bulk composition prediction was validated using SEM-EDX and wet chemical analysis. The non-ideal solution model was then applied to predict the composition of the dust generated during EML testing. The thicknesses of the deposited layer on the EML coil at various locations were also calculated using the geometry of the facility and results were validated with near-real-time dust layer predictions from toxicity tracking software developed by the German Space Center (DLR) Microgravity User Support Center (MUSC).
LiNbO3 (LNO) is a material suitable for high-frequency and wideband RF filters as well as photonic appli-cations due to its outstanding piezoelectric and optical properties. Applications such as thin-film bulk acoustic wave resonators or highly confined electro-optic modulators require thin films, which are still challenging to be obtained with the necessary crystalline quality by deposition methods. Alternatively to deposition, crystal ion-slicing (CIS) or Smart CutTM enables obtaining thin films hundreds of nanome-ters thick from the bulk single-crystal utilizing high-energy and dose implantation of light atoms. The price to pay is the partial degradation of the initial crystalline perfection, which translates to a degrada-tion of the piezoelectric performance of the material if the CIS-induced damage is not eliminated.This work aims to understand the physics of the recrystallization process of the CIS-damaged LNO crys-tal upon thermal annealing. The study of the coherent and diffuse scattering by high-resolution X-ray diffraction, complemented by micro-Raman backscattering spectroscopy and Transmission Electron Microscopy (TEM), allowed to study the recovery of the crystallinity from the CIS-induced lattice strain and stress and the progressive reduction of the defects clusters dimension.& COPY; 2023 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
In this work, we demonstrate that highly oriented c-axis aluminium scandium nitride (AlScN) piezoelectric thin films can be deposited via microwave plasma-assisted reactive high power impulse magnetron sputtering (MARHiPIMS), without the necessity of substrate heating. A combination of in situ plasma diagnostics, i.e. time-offlight mass spectrometry (ToF-MS), modified quartz crystal microbalance (m-QCM), and magnetic field measurements allowed to optimise the deposition conditions, in turn maximising the nitrogen supply and ionic flux at the substrate region, while maintaining stable discharge conditions. The AlScN thin films synthesised in this study were deposited as chemically gradient coatings with varying levels of scandium doping, and were characterised using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). Obtaining highly textured films was made possible with the addition of microwave plasma to the optimised HiPIMS discharge, where the wurtzite AlScN films (with up to 20 at. % Sc) exhibited a stronger texture in the (0002) orientation compared to films prepared without microwave plasma. Additionally, the use of a microwave plasma led to a significant decrease in oxygen content in the films and increase in nitrogen content, ensuring stoichiometric compositions. Based on the results mentioned above, it is expected that the AlScN thin films fabricated via MAR-HiPIMS would exhibit a strong piezoelectric response.
This work focuses on the low temperature fabrication process of InN thin films via microwave plasma-assisted reactive high power impulse magnetron sputtering (MAR-HiPIMS). The influence of microwave plasma on the HiPIMS discharge process at various nitrogen flows and microwave powers was monitored and characterised through in situ diagnostics, including following HiPIMS I(V,t) curves, optical emission spectroscopy (OES), as well as performing time-resolved Langmuir probe and time-of-flight mass spectroscopy (ToF-MS) measurements. This was followed by the deposition of InN films via standard reactive HiPIMS (reference sample) and MAR-HiPIMS and their characterisation via X-ray diffraction (XRD), reflectometry (XRR), as well as scanning and transmission electron microscopy (SEM, TEM). It was found that the microwave plasma facilitates the dissoci-ation/activation of nitrogen species and supplies seed electrons to the magnetron discharge plasma. Furthermore, the energy of the incoming ions was determined via ToF-MS, and it was possible to identify their plasma origin and temporal behaviour. The produced R-HiPIMS sample was highly metallic, with no nitride phase detected. The MAR-HiPMS film, however, was stoichiometric and exhibited (0002) direction texturing, with an optical bandgap of approx. 1.5 eV, electron concentration of 2.72 x 1020 cm -3 and electron mobility of 7.16 cm2V- 1s- 1 (in the range for polycrystalline InN).
Thermoplastic extrusion based additive manufacturing (MEX-AM), is a very interesting fabrication method for the shaping of larger ceramic parts. Commercial filaments are currently available in the market, but due to the lack of information from the suppliers, it is not easy to select the suitable filament material for the 3D printing of individual ceramic objects. In this study, three commercial yttria-stabilized zirconia (YSZ) filaments provided by Fabru GmbH, SiCeram GmbH and PT+A GmbH were investigated. According to our results, it is possible to print YSZ filaments with extremely different flexibility and rheological properties. Compared to the other two fila-ments, the Fabru filament resulted in significantly higher flexibility, but the extrusion pressure to print it through a 0.25 mm nozzle was significantly higher at 150 degrees C. Interestingly, in the SiCeram filament, a grain orientation effect could be observed. Based on STA analysis it can be assumed that for the Fabru filament, the polymer which decomposes at a high temperature can already be removed by solvent debinding (SD). Finally, 70 mm tall cup structure including overhang features and different wall thicknesses was used to evaluate the printing and post -processing of YSZ filaments.
In thin film deposition processes, the lower limit of the deposition temperature is determined by the used coating technology and the duration of the coating process and is usually higher than room temperature. Hence, the processing of thermally sensitive materials and the adjustability of thin film morphology are limited. In consequence, for factual low-temperature deposition processes, an active cooling of the substrate is required. The effect of low substrate temperature on thin film properties during ion beam sputtering was investigated. The SiO2 and Ta2O5 films grown at 0°C show a trend of lower optical losses and higher laser induced damage threshold (LIDT) compared to 100°C.
Metal-Organic Frameworks (MOFs) are extended three-dimensional metal-organic clusters created by the self -assembly of metal ions with organic ligands, whose repeated unit spreads in space very orderly. Yttrium based 3D network structure, have been synthesized using the tritopic organic linker 1,3,5-benzenetricarboxylic acid (H3-BTC) adopting a one-pot, green approach through a fine tuning of the process parameters like tem-perature and time. The syntheses have been carried out at various temperatures and reaction times, in order to correlate the morphological and structural features to the synthetic conditions. The synthesized Y-BTC samples have been studied in detail through powder X-ray diffraction (PXRD) and FT-IR spectroscopy in order to analyse the 3D structure arrangements. Specifically, the Y-BTC PXRD patterns have been compared with patterns derived from literature data. The Y-BTC sample synthesized at room temperature for 24 h has the same structure of the known Y(BTC)(H2O)6 compound, while the Y-BTC produced at high temperature for 24 h has a new structure, whose cell parameters are a = 14.668(2) angstrom, b = 16.316(2) angstrom, and c = 6.9650(4) angstrom. Field emission scanning electron microscopy (FE-SEM) has allowed to investigate the morphological evolution of the MOF as a function of operative parameters. Additionally, thermal analyses (TGA and DSC) have assessed the thermal stability and structural modifications of the Y-BTC samples.
Thin film layer-by-layer room-temperature synthesis of targeted DUT-8 MOFs from 2,6-ndc and dabco ligands give different crystalline framework growths depending on the metal cation used: Cu(2,6-ndc) and Zn(2,6-ndc)(H2O).
Biocompatible polymer films demonstrating excellent thermal stability are highly desirable for high-temperature (>250 °C) applications, especially in the bioelectronic encapsulation domain. Parylene, as an organic thin film, is a well-established polymer material exhibiting excellent barrier properties and is often the material of choice for biomedical applications. This work investigated the thermal impact on the bulk properties of four types of parylene films: parylene N, C, VT4, and AF4. The films, deposited using the standard Gorham process, were analyzed at varying annealing temperatures from room temperature up to 450 °C. Thermal properties were identified by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) methods, while X-ray diffraction (XRD) analysis showed the effect of high-temperature exposure on the structural properties. In addition to thermal and structural analysis, the barrier properties were measured through the helium transmission rate (HTR) and the water vapor transmission rate (WVTR). Fluorinated parylene films were confirmed to be exceptional materials for high-temperature applications. Parylene AF4 film, 25um thick, demonstrated excellent barrier performance after 300 °C exposure, with an HTR and a WVTR of 12.18 × 103 cm3 (STP) m−2 day−1 atm−1 and 6.6 g m−2 day−1, respectively.
High-entropy materials are compositionally complex materials which often contain five or more elements. The most commonly studied materials in this field are alloys and oxides, where their composition allows for tunable materials properties. High-entropy layered double hydroxides have been recently touted as the next focus for the field of high-entropy materials to expand into. However, most previous work on multi-cationic layered double hydroxides has focused on syntheses with 5 or less cations in the structure. To bridge this gap into high-entropy materials, this work explores the range and extent of different compositional combinations for high-entropy double layered hydroxides. Specifically, pure layered double hydroxides were synthesized with different combinations of 7 cations (Mg, Co, Cu, Zn, Ni, Al, Fe, Cr) as well as one combination of 8 cations by utilizing a hydrothermal synthesis method. Furthermore, magnetic properties of the 8-cation LDH were investigated.
Fe-Mn-Si shape memory alloys are materials, whose functional properties strongly depend on microstructural factors such as grain size and orientation, phase fraction and chemical composition. The present study demonstrates the possibility of microstructure modification via process parameter variation on a Fe-Mn-Si based shape memory alloy fabricated by laser powder bed fusion. By varying the scan speed, samples characterized by coarse elongated grains with strong <001> orientation along the build direction or by finer equiaxed grains without preferential orientation can be fabricated. Changes in the volume phase fraction of bcc-δ ferrite and fcc-γ austenite are also introduced by selective Mn evaporation. A direct correlation between the generated microstructure and achieved mechanical and shape memory properties is found.
Electrospun nanofibers have shown great potential as drug vehicles and tissue engineering scaffolds. However, the successful encapsulation of multiple hydrophilic/hydrophobic therapeutic compounds is still challenging. Herein, sodium alginate/poly(ε-caprolactone) core/shell nanofibers were fabricated via water-in-oil emulsion electrospinning. The sodium alginate concentration, water-to-oil ratio, and surfactant concentration were optimized for the maximum stability of the emulsion. The results demonstrated that an increasing water-to-oil ratio results in more deviation from Newtonian fluid and leads to a broader distribution of the fibers' diameters. Moreover, increasing poly(ε-caprolactone) concentration increases loss and storage moduli and increases the diameter of the resulting fibers. The nanofibers' characteristics were investigated by scanning electron microscopy, transmission electron microscopy, confocal laser scanning microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and water contact angle measurements. It was observed that using an emulsion composition of 10% (w/v) PCL and a water-to-oil ratio of 0.1 results in smooth, cylindrical, and uniform core/shell nanofibers with PCL in the shell and ALG in the core. The in vitro cell culture study demonstrated the favorable biocompatibility of nanofibers. Overall, this study provides a promising and trustworthy material for biomedical applications.
Advanced methods such as high-resolution X-ray diffraction and X-ray micro CT allow highly precise determination of materials' residual stress, volume, and lattice defects. Their conjoint exploitation offers a powering tool to facilitate the industrial implementation of novelties in microfabrication. The wafer-level packaging represents a critical step of the MEMS microfabrication resulting in a hermetic, defect-and stress-free interface. For the first time, such critical parameters are investigated related to a novel wafer-bonding process, namely Impulse Current Bonding (ICB), and compared to the standard anodic bonding technology used for MEMS production. The ICB does not induce any relevant residual stress at the interface above the limit of 1 MPa, determined by the unrivaled strain detectability of HRXRD. The bonding interface is devoid of any defects, as defined by X-ray micro-CT studies. The ICB technology reduces the thermal budget of the packaging up to 85% compared to the anodic bonding, which outlines an outstanding step forward in reducing the energy footprint. The extension of ICB to other materials systems such as glass to ceramic or metals makes this technology a promising candidate for numerous applications, including the design of biocompatible devices for bio-implants.
The reliability of semiconductor materials with electrical and optical properties are connected to their structures. The elastic strain field and tilt analysis of the crystal lattice, detectable by the variation in position and shape of the diffraction peaks, is used to quantify defects and investigate their mobility. The exploitation of high-resolution X-ray diffraction-based methods for the evaluation of structural defects in semiconductor materials and devices is reviewed. An efficient and non-destructive characterization is possible for structural parameters such as, lattice strain and tilt, layer composition and thickness, lattice mismatch, and dislocation density. The description of specific experimental diffraction geometries and scanning methods is provided. Today's X-ray diffraction based methods are evaluated and compared, also with respect to their applicability limits. The goal is to understand the close relationship between lattice strain and structural defects. For different material systems, the appropriate analytical methods are highlighted.
Most of the natural or fabricated fibrous materials exhibit multiscale structures, which critically influence their mechanical, optical, and electronic properties.Therefore, knowing the structure is important to steer the properties or design novel fibrous material.This requires multiscale structural characterization to enrich their structure-properties relationship.State-of-the-art small-angle X-ray scattering (SAXS) and wide-angle X-ray diffraction (WAXD) techniques are extremely powerful to characterize such materials from the nanometer to the Ångström scale [1].