ABSTRACT
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.
ABSTRACT
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.
ABSTRACT
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.
ABSTRACT
The evolution of phase separation and ordering processes determines the structure and properties of Ni-based superalloys. Here we use atom probe tomography to clarify the origin of γ particles occurring in ordered (L12) γ' precipitates in a Ni86.1Al8.5Ti5.4 alloy. Particularly, we elucidate the evolution from nanoscaled Ni-rich heterogeneities (Ni-rich clusters) to γ spheres and then γ plates inside γ' precipitates from the compositional and the thermodynamic point of view. We find that Ni supersaturation of γ' precipitates is relieved by formation of Ni-rich clusters, which results in an energetically more favorable state. Subsequently, coalescence introduces necking between the Ni-rich clusters and leads to the formation of γ particles. Our results demonstrate that phase separation of γ' precipitates is characterized by different stages with various governing driving forces.
ABSTRACT
Semi-conducting nanocrystals embedded in a non-conducting matrix of silicate glass may be used as non-volatile data storage device. Structures of silicate glasses are conveniently produced by a sol-gel process, which offers the possibility to coat tip-shaped substrates with a silica layer. The study presents first results of their local chemical analysis by laser-assisted atom probe. Till date the exact mechanisms of laser pulsing are still controversial. But it is common sense that there is an at least considerable heating effect on the tip, which leads to a short temperature rise and a prolonged cooling period in materials of low heat conductivity. This effect alters the shape of mass peaks and is examined here using a one-dimensional model of heat transport.
ABSTRACT
Currently atom probe tomography provides the highest spatial resolution compared to all other volume analysis techniques. Owing to its single atom sensitivity, it is specially suited to study nano-structured materials. Therefore, a new atom probe was installed at the Institute for Material Physics at University of Muenster, Germany, to study thin film reactions. Since the available budget was rather limited, a cost-effective non-commercial atom probe was constructed. The instrument is based on a 2D delay line detector system of 120 mm diameter. To achieve a large collecting angle and thus large volumes of analysis, a straight flight tube without a reflectron is used. This way, the flight distance may be reduced down to 160 mm. However, the variable chamber layout allows using a reflectron as an alternative. Furthermore, a laser system is implemented that delivers pulses in the 500 ps range to make possible laser-assisted evaporation of atoms. The article describes instrumental details and presents first characteristic data.
