scholarly journals 3D sub-nanometer analysis of glucose in an aqueous solution by cryo-atom probe tomography

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
T. M. Schwarz ◽  
C. A. Dietrich ◽  
J. Ott ◽  
E. M. Weikum ◽  
R. Lawitzki ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Density Functional ◽  
Chemical Characterization ◽  
Analytical Techniques ◽  
Atom Probe ◽  
Characterization Methods ◽  
Signal Deconvolution ◽  
The Stability ◽  
Frozen Solutions ◽  
3D Volume

AbstractAtom 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.

scholarly journals 3D Sub-Nanometer Analysis of Glucose in an Aqueous Solution by Cryo-Atom Probe Tomography

2021 ◽  
Author(s):  
Tim Schwarz ◽  
Carolin Dietrich ◽  
Jonas Ott ◽  
Eric Weikum ◽  
Robert Lawitzki ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Density Functional ◽  
Chemical Characterization ◽  
Analytical Techniques ◽  
Atom Probe ◽  
Biological Molecules ◽  
Characterization Methods ◽  
Signal Deconvolution ◽  
The Stability ◽  
Frozen Solutions

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 and spatial resolution capabilities as a step toward the measurement of biological molecules in solution in 3D with sub-nanometre resolution by using cryo-APT. Our analyses take analytical techniques to a new level, since chemical characterization methods for cryogenically-frozen solutions or biological materials are limited.

Atom-probe tomography of surface oxides and oxidized grain boundaries in alloys from nuclear reactors

2013 ◽  
Vol 1514 ◽  
pp. 107-118 ◽  
Author(s):  
Karen Kruska ◽  
David W Saxey ◽  
Takumi Terachi ◽  
Takuyo Yamada ◽  
Peter Chou ◽  
...  
Keyword(s):  
Grain Boundary ◽  
Grain Boundaries ◽  
Atom Probe Tomography ◽  
Nuclear Reactors ◽  
Bulk Material ◽  
Chemical Characterization ◽  
Atom Probe ◽  
Aqueous Environment ◽  
Pressurized Water ◽  
Surface Oxides

ABSTRACTThe preparation of site-specific atom-probe tomography (APT) samples containing localized features has become possible with the use of focused ion beams (FIBs). This technique was used to achieve the analysis of surface oxides and oxidized grain boundaries in this paper. Transmission electron microscopy (TEM), providing microstructural and chemical characterization of the same features, has also been used, revealing crucial additional information.The study of grain boundary oxidation in stainless steels and nickel-based alloys is required in order to understand the mechanisms controlling stress corrosion cracking in nuclear reactors. Samples oxidized under simulated pressurized water reactor primary water conditions were used, and FIB lift-out TEM and APT specimens containing the same oxidized grain boundary were prepared and fully characterized. The results from both techniques were found fully consistent and complementary.Chromium-rich spinel oxides grew at the surface and into the bulk material, along grain boundaries. Nickel was rejected from the oxides and accumulated ahead of the oxidation front. Lithium, which was present in small quantities in the aqueous environment during oxidation, was incorporated in the oxide. All phases were accurately quantified and the effect of different experimental parameters were analysed.

Direct observation of incommensurate structure in Mo3Si

2016 ◽  
Vol 72 (6) ◽  
pp. 660-666 ◽  
Author(s):  
Ahmet Gulec ◽  
Xiaoxiang Yu ◽  
Matthew Taylor ◽  
John H. Perepezko ◽  
Laurence Marks
Keyword(s):  
Crystal Structure ◽  
Density Functional Theory ◽  
Atom Probe Tomography ◽  
Density Functional ◽  
Density Functional Theory Calculations ◽  
Atom Probe ◽  
Atomic Resolution ◽  
Contrast Imaging ◽  
Functional Theory ◽  
Incommensurate Structure

Z-contrast imaging, electron diffraction, atom-probe tomography (APT) and density functional theory calculations were used to study the crystal structure of the Mo3Si phase which was previously reported to have an A15 crystal structure. The results showed that Mo3Si has an incommensurate crystal structure with a non-cubic unit cell. The small off-stoichiometry in composition of the sample which was revealed by APT and atomic resolutionZ-contrast imaging suggested that site substitution caused the development of split atomic positions, disorder and vacancies.

Impact of Carbon on Threshold Voltage Shift in MOSFET Studied by 3D Atom Probe Tomography

2017 ◽  
Author(s):  
Ju-Heon Kim ◽  
Euna Ok ◽  
Hyunmi Sim ◽  
Dongkeun Na ◽  
Ho Seok Song ◽  
...  
Keyword(s):  
Threshold Voltage ◽  
Atom Probe Tomography ◽  
Analytical Techniques ◽  
Gate Oxide ◽  
Atom Probe ◽  
Single Atom ◽  
Device Performance ◽  
Si Substrate ◽  
Threshold Voltage Shift ◽  
Voltage Shift

Abstract In this paper, impact of carbon on threshold voltage in MOSFET-based device is studied by 3D-atom probe tomography (APT). Carbon is one of most difficult contaminants incorporated from fab-environment to be detected by typical analytical techniques such as TEM-EDS or SIMS. Here, we successfully demonstrated the detection of carbon segregated at gate oxide/Si substrate interface using 3D-APT with single-atom sensitivity and sub-nanometer spatial resolution. It was found that the carbon contaminants have significant effect on the threshold voltage shift (ΔVth), in which ΔVth increases slightly with increasing carbon concentration. The deterioration of device performance is explained by means of which the positively ionized carbons at the interface acting as additional positive charges affecting the inversion to n-channel.

Atom Probe Tomography: Studying Reactions on Top of the Tip

2006 ◽  
Vol 46 ◽  
pp. 126-135 ◽  
Author(s):  
Guido Schmitz ◽  
Constantin Ene ◽  
Ch. Lang ◽  
Vitaliy Vovk
Keyword(s):  
Solid State ◽  
Atom Probe Tomography ◽  
Atom Probe ◽  
Modern Technology ◽  
Solid State Reactions ◽  
Reactive Diffusion ◽  
Atomic Transport ◽  
The Stability ◽  
Gmr Sensor ◽  
Detection And Localization

Down-scaling is a major principle of modern technology. As a consequence, the stability of many technical devices is controlled by solid state reactions that proceed on the range of a few nanometres only. On such a short length scale even basic aspects of reaction physics as fundamental as e.g. the Ficks laws of diffusion, need to be reconsidered. Only very few dedicated techniques are suitable to study atomic transport and reactions with sufficient accuracy. Among them, the atom probe tomography is exceptional, as it allows the detection and localization of individual atoms with an accuracy of a lattice constant. An almost complete reconstruction of the 3D atomic arrangement of different atomic species gets possible. This article provides an overview on recent atom probe studies of reactive diffusion. After an introduction into the principles of the analysis method, physical mechanisms of solid state reactions are discussed in view of recent experiments at metallic thin film interfaces. How does nucleation of an interfacial product take place? In which way do grain boundaries influence the reaction? As a technical example, the stability of Cu/NiFe GMR sensor layers is discussed.

Atom Probe Tomography: A Technique for Nanoscale Characterization

2004 ◽  
Vol 10 (3) ◽  
pp. 336-341 ◽  
Author(s):  
M.K. Miller ◽  
E.A. Kenik
Keyword(s):  
Atom Probe Tomography ◽  
Analytical Techniques ◽  
Size Composition ◽  
Oxide Dispersion Strengthened ◽  
Atom Probe ◽  
Oxide Dispersion ◽  
Mechanically Alloyed ◽  
Nanoscale Characterization ◽  
Tomography Data

Atom probe tomography is a technique for the nanoscale characterization of microstructural features. Analytical techniques have been developed to estimate the size, composition, and other parameters of features as small as 1 nm from the atom probe tomography data. These methods are outlined and illustrated with examples of yttrium-, titanium-, and oxygen-enriched particles in a mechanically alloyed, oxide-dispersion-strengthened steel.

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