Correlative atomic force microscopy and scanning electron microscopy of bacteria-diamond-metal nanocomposites.

Research investigating the interface between biological organisms and nanomaterials nowadays requires multi-faceted microscopic methods to elucidate the interaction mechanisms and effects. Here we describe a novel approach and methodology correlating data from an atomic force microscope inside a scanning electron microscope (AFM-in-SEM). This approach is demonstrated on bacteria-diamond-metal nanocomposite samples relevant in current life science research. We describe a procedure for preparing such multi-component test samples containing E. coli bacteria and chitosan-coated hydrogenated nanodiamonds decorated with silver nanoparticles on a carbon-coated gold grid. Microscopic topography information (AFM) is combined with chemical, material, and morphological information (SEM using SE and BSE at varied acceleration voltages) from the same region of interest and processed to create 3D correlative probe-electron microscopy (CPEM) images. We also establish a novel 3D RGB color image algorithm for merging multiple SE/BSE data from SEM with the AFM surface topography data which provides additional information about microscopic interaction of the diamond-metal nanocomposite with bacteria, not achievable by individual analyses. The methodology of CPEM data interpretation is independently corroborated by further in-situ (EDS) and ex-situ (micro-Raman) chemical characterization as well as by force volume AFM analysis. We also discuss the broader applicability and benefits of the methodology for life science research.

Microstructure and Mechanical Properties of Spark Plasma Sintered CoCrFeNiNbX High-Entropy Alloys with Si Addition.

Three mechanically alloyed (MA) and spark plasma sintered (SPS) CoCrFeNiNbX (X = 5, 20, and 35 at.%) alloys with an addition of 5 at.% of SiC were investigated. The face-centered cubic (FCC) high-entropy solid solution, NbC carbides, and hexagonal Laves phase already developed during MA. In addition, the SPS compacting led to the formation of oxide particles in all alloys, and the Cr7C3 carbides in the Nb5 alloy. The fraction of the FCC solid solution decreased with increasing Nb concentration at the expense of the NbC carbide and the Laves phase. Long-term annealing at 800 °C led to the disappearance of the Cr7C3 carbide in the Nb5 alloy, and new oxides-Ni6Nb6O, Cr2O3, and CrNbO4-were formed. At laboratory temperature, the Nb5 alloy, containing only the FCC matrix and carbide particles, was relatively strong and very ductile. At a higher Nb content (Nb20 and Nb35), the alloys became brittle. After annealing for 100 h at 800 °C, the Nb5 alloy conserved its plasticity and the Nb20 and Nb35 alloys maintained or even increased their brittleness. When tested at 800 °C, the Nb5 and Nb20 alloys deformed almost identically (CYS ~450 MPa, UTS ~500 MPa, plasticity ~18%), whereas the Nb35 alloy was much stronger (CYS of 1695 MPa, UCS of 1817 MPa) and preserved comparable plasticity.

Interface-Driven Strain in Heavy Ion-Irradiated Zr/Nb Nanoscale Metallic Multilayers: Validation of Distortion Modeling via Local Strain Mapping.

Nanolayered metallic alloys are promising materials for nuclear applications thanks to their resistance to radiation damage. Here, we investigate the effect of ion (C, Si, and Cu) irradiation at room temperature with different fluences into sputtered Zr/Nb metallic multilayer films with periods 27 nm (thin) and 96 nm (thick). After irradiation, while a high strain in the entire thin nanoscale metallic multilayer (NMM) is observed, a quite small strain in the entire thick NMM is established. This difference is further analyzed by a semianalytical model, and the reasons behind it are revealed, which are also validated by local strain mapping. Both methods show that within a thick layer, two opposite distortions occur, making the overall strain small, whereas in a thin layer, all the atomic planes are affected by the interface and are subjected to only a single type of distortion (Nb─tension and Zr─compression). In both thin and thick NMMs, with increasing damage, the strain around the interface increases, resulting in a release of the elastic energy at the interface (decrease in the lattice mismatch), and the radiation-induced transition of the Zr/Nb interfaces from incoherent to partially coherent occurs. Density functional theory simulations decipher that the inequality of point defect diffusion flux from the inner to the interface-affected region is responsible for the presence of opposite distortions within a layer. Technologically, based on this work, we estimated that Zr/Nb55 with thicknesses around Zr = 24 nm and Nb = 31 nm is the most promising multilayer system with the high radiation damage resistance and minimum swelling for nuclear applications.

Indentation Size Effect in CoCrFeMnNi HEA Prepared by Various Techniques.

High entropy alloys (HEAs) are materials of great application potential and which have been extensively studied during the last two decades. As the number of possible element combinations is enormous, model materials representing certain groups of HEAs are used for the description of microstructure, properties, and deformation mechanisms. In this study, the microstructure and mechanical properties of the so-called Cantor alloy composed of Co, Cr, Fe, Mn, and Ni in equiatomic ratios prepared by various techniques (casting, melt-spinning, spark plasma sintering) were examined. The research focused on the indentation measurements, namely, the indentation size effect describing the evolution of the hardness with penetration depth. It was found that the standard Nix-Gao model can be used for this type of alloy at higher penetration depths and its parameters correlate well with microstructural observations. The Nix-Gao model deviates from the measured data at the submicrometer range and the applied modification affords additional information on the deformation mechanism.

Effect of Initial Powders on Properties of FeAlSi Intermetallics.

FeAlSi intermetallics are materials with promising high-temperature mechanical properties and oxidation resistance. Nevertheless, their production by standard metallurgical processes is complicated. In this study, preparation of powders by mechanical alloying and properties of the samples compacted by spark plasma sintering was studied. Various initial feedstock materials were mixed to prepare the material with the same chemical composition. Time of mechanical alloying leading to complete homogenization of powders was estimated based on the microstructure observations, results of XRD and indentation tests. Microstructure, phase composition, hardness and fracture toughness of sintered samples was studied and compared with the properties of powders before the sintering process. It was found that independently of initial feedstock powder, the resulting phase composition was the same (Fe3Si + FeSi). The combination of hard initial powders required the longest milling time, but it led to the highest values of fracture toughness.