RESUMO
Atom Probe Tomography (APT) is currently a well-established technique to analyse the composition of solid materials including metals, semiconductors and ceramics with up to near-atomic resolution. Using an aqueous glucose solution, we now extended the technique to frozen solutions. While the mass signals of the common glucose fragments CxHy and CxOyHz overlap with (H2O)nH from water, we achieved stoichiometrically correct values via signal deconvolution. Density functional theory (DFT) calculations were performed to investigate the stability of the detected pyranose fragments. This paper demonstrates APT's capabilities to achieve sub-nanometre resolution in tracing whole glucose molecules in a frozen solution by using cryogenic workflows. We use a solution of defined concentration to investigate the chemical resolution capabilities as a step toward the measurement of biological molecules. Due to the evaporation of nearly intact glucose molecules, their position within the measured 3D volume of the solution can be determined with sub-nanometre resolution. Our analyses take analytical techniques to a new level, since chemical characterization methods for cryogenically-frozen solutions or biological materials are limited.
RESUMO
Measuring biological samples by atom probe tomography (APT) in their natural environment, i.e. aqueous solution, would take this analytical method, which is currently well established for metals, semi-conductive materials and non-metals, to a new level. It would give information about the 3D chemical structure of biological systems, which could enable unprecedented insights into biological systems and processes, such as virus protein interactions. For this future aim, we present as a first essential step the APT analysis of pure water (Milli-Q) which is the main component of biological systems. After Cryo-preparation, nanometric water tips are field evaporated with assistance by short laser pulses. The obtained data sets of several tens of millions of atoms reveal a complex evaporation behavior. Understanding the field evaporation process of water is fundamental for the measurement of more complex biological systems. For the identification of the individual signals in the mass spectrum, DFT calculations were performed to prove the stability of the detected molecules.
RESUMO
Thermally-activated phase transitions in Pt/Mn/Fe thin films were investigated by a combination of x-ray diffraction, transmission electron microscopy, secondary neutral mass spectrometry depth profiling, atomic force microscopy, and magnetic properties measurements. Post-annealing was carried out in vacuum to different temperatures up to 620 °C. Initially, at temperatures between 280 °C-450 °C first L10-MnPt is formed at the Mn/Pt interface followed by the most likely formation of metastable bcc Fe3Pt, which gets transformed by further annealing to fcc Fe3Pt and eventually to chemically ordered L12-Fe3Pt. The final product after annealing at 620 °C consists of two interesting phases, which are relevant for spintronic applications, antiferromagnetic L10-MnPt with addition of Fe and ferromagnetic L12-Fe3Pt, consistent with the initial element composition.
RESUMO
The fast Li conductivity of LiBH4 envisages its use in all-solid-state batteries. Powders are commonly applied. But here, we study the formation of dense micrometer films by melting, spinning and subsequent solidifying. Characterized by electron microscopy, and spectroscopy (EDX/XPS/impedance), a reversible phase transformation is confirmed as well as a maximum conductivity of 103 S cm-1.
