scholarly journals Nanoscale Stoichiometric Analysis of a High-Temperature Superconductor by Atom Probe Tomography

2017 ◽  
Vol 23 (2) ◽  
pp. 414-424 ◽  
Author(s):  
Stella Pedrazzini ◽  
Andrew J. London ◽  
Baptiste Gault ◽  
David Saxey ◽  
Susannah Speller ◽  
...  
Keyword(s):  
High Temperature ◽  
Atom Probe Tomography ◽  
High Temperature Superconductor ◽  
Analytical Techniques ◽  
Atom Probe ◽  
Three Dimensions ◽  
Oxygen Stoichiometry ◽  
Superconducting Properties ◽  
Experimental Conditions ◽  
Wide Range

AbstractThe functional properties of the high-temperature superconductor Y1Ba2Cu3O7−δ(Y-123) are closely correlated to the exact stoichiometry and oxygen content. Exceeding the critical value of 1 oxygen vacancy for every five unit cells (δ>0.2, which translates to a 1.5 at% deviation from the nominal oxygen stoichiometry of Y7.7Ba15.3Cu23O54−δ) is sufficient to alter the superconducting properties. Stoichiometry at the nanometer scale, particularly of oxygen and other lighter elements, is extremely difficult to quantify in complex functional ceramics by most currently available analytical techniques. The present study is an analysis and optimization of the experimental conditions required to quantify the local nanoscale stoichiometry of single crystal yttrium barium copper oxide (YBCO) samples in three dimensions by atom probe tomography (APT). APT analysis required systematic exploration of a wide range of data acquisition and processing conditions to calibrate the measurements. Laser pulse energy, ion identification, and the choice of range widths were all found to influence composition measurements. The final composition obtained from melt-grown crystals with optimized superconducting properties was Y7.9Ba10.4Cu24.4O57.2.

scholarly journals Reflections on the Analysis of Interfaces and Grain Boundaries by Atom Probe Tomography

2020 ◽  
Vol 26 (2) ◽  
pp. 247-257 ◽  
Author(s):  
Benjamin M. Jenkins ◽  
Frédéric Danoix ◽  
Mohamed Gouné ◽  
Paul A.J. Bagot ◽  
Zirong Peng ◽  
...  
Keyword(s):  
Grain Boundaries ◽  
Atom Probe Tomography ◽  
Compositional Analysis ◽  
Atom Probe ◽  
Atomic Scale ◽  
Three Dimensions ◽  
Specimen Preparation ◽  
Structure Property ◽  
Wide Range

AbstractInterfaces play critical roles in materials and are usually both structurally and compositionally complex microstructural features. The precise characterization of their nature in three-dimensions at the atomic scale is one of the grand challenges for microscopy and microanalysis, as this information is crucial to establish structure–property relationships. Atom probe tomography is well suited to analyzing the chemistry of interfaces at the nanoscale. However, optimizing such microanalysis of interfaces requires great care in the implementation across all aspects of the technique from specimen preparation to data analysis and ultimately the interpretation of this information. This article provides critical perspectives on key aspects pertaining to spatial resolution limits and the issues with the compositional analysis that can limit the quantification of interface measurements. Here, we use the example of grain boundaries in steels; however, the results are applicable for the characterization of grain boundaries and transformation interfaces in a very wide range of industrially relevant engineering materials.

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.

Challenges Associated with the Characterisation of Nanocrystalline Materials Using Atom Probe Tomography

2010 ◽  
Vol 654-656 ◽  
pp. 2366-2369 ◽  
Author(s):  
Feng Zai Tang ◽  
Talukder Alam ◽  
Michael P. Moody ◽  
Baptiste Gault ◽  
Julie M. Cairney
Keyword(s):  
Quantitative Analysis ◽  
Atom Probe Tomography ◽  
Nanocrystalline Materials ◽  
Atom Probe ◽  
Atomic Scale ◽  
Three Dimensions ◽  
Specimen Preparation ◽  
Compositional Information

Atom probe tomography provides compositional information in three dimensions at the atomic scale, and is therefore extremely suited to the study of nanocrystalline materials. In this paper we present atom probe results from the investigation of nanocomposite TiSi¬Nx coatings and nanocrystalline Al. We address some of the major challenges associated with the study of nanocrystalline materials, including specimen preparation, visualisation, common artefacts in the data and approaches to quantitative analysis. We also discuss the potential for the technique to relate crystallographic information to the compositional maps.

Functionalization of Graphene with O and S for Catalytic Degradation of Chlorophenols and Dyes

2021 ◽  
Vol 1019 ◽  
pp. 194-204
Author(s):  
S. Sudhaparimala ◽  
R. Usha
Keyword(s):  
Graphene Oxide ◽  
Organic Dyes ◽  
Analytical Techniques ◽  
Degradation Process ◽  
Experimental Conditions ◽  
Photocatalytic Application ◽  
Wide Range ◽  
Doped Graphene ◽  
The Given ◽  
Graphene Structures

Graphene, functionalized with the heteroatoms like nitrogen, oxygen and sulphur atoms has been well explored for a wide range of applications but only few reports are available on its adsorption and photocatalytic application in the degradation of chlorophenols and organic dyes. A simple and energy-efficient process to prepare graphene oxide and sulphur doped graphene oxide was developed. The micro structure and surface morphology were confirmed by the analytical techniques of Powder X-ray diffractogram (PXRD), Fourier Transformed Raman Spectroscopy (FT-Raman), Scanning Electron Microscopy. The results were suggestive of the structures suitable for screening their catalytic activity in the degradation of the highly toxic polychlorophenols and organic dyes. The adsorption and photo catalytic properties of the asprepared samples were screened for the degradation process and it was found that sulphur doped graphene oxide showed more positive results for the degradation of chlorophenols than graphene oxide. Under the given experimental conditions the decoloration of dyes were not satisfactory. Ultimately, the study provided an economical and efficient, method for tuning graphene structures for the removal of pollutants in wastewater.

scholarly journals A Gas-Phase Reaction Cell for Modern Atom Probe Systems

2019 ◽  
Vol 25 (2) ◽  
pp. 410-417 ◽  
Author(s):  
Daniel Haley ◽  
Ingrid McCarroll ◽  
Paul A. J. Bagot ◽  
Julie M. Cairney ◽  
Michael P. Moody
Keyword(s):  
Gas Phase ◽  
Atom Probe Tomography ◽  
Atom Probe ◽  
Phase Reaction ◽  
Reaction Cell ◽  
Current Form ◽  
Gas Phase Reaction ◽  
Wide Range ◽  
Gas Interactions ◽  
Selection Of

AbstractIn this work, we demonstrate a new system for the examination of gas interactions with surfaces via atom probe tomography. This system provides capability of examining the surface and subsurface interactions of gases with a wide range of specimens, as well as a selection of input gas types. This system has been primarily developed to aid the investigation of hydrogen interactions with metallurgical samples, to better understand the phenomenon of hydrogen embrittlement. In its current form, it is able to operate at pressures from 10−6 to 1000 mbar (abs), can use a variety of gasses, and is equipped with heating and cryogenic quenching capabilities. We use this system to examine the interaction of hydrogen with Pd, as well as the interaction of water vapor and oxygen in Mg samples.

scholarly journals Complementary Atom Probe Tomography and Electron Microscopy of Oxidation of Ni-Base Alloys in High-Temperature Water Environments

2013 ◽  
Vol 19 (S2) ◽  
pp. 970-971 ◽  
Author(s):  
D.K. Schreiber ◽  
M.J. Olszta ◽  
S.M. Bruemmer
Keyword(s):  
Electron Microscopy ◽  
High Temperature ◽  
Atom Probe Tomography ◽  
Atom Probe ◽  
High Temperature Water ◽  
Temperature Water

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

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.

Characterization of Nanoporous Materials with Atom Probe Tomography

2015 ◽  
Vol 21 (3) ◽  
pp. 557-563 ◽  
Author(s):  
Björn Pfeiffer ◽  
Torben Erichsen ◽  
Eike Epler ◽  
Cynthia A. Volkert ◽  
Piet Trompenaars ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
Nanoporous Materials ◽  
Three Dimensions ◽  
Chemical Information ◽  
Nanoporous Material ◽  
Open Cell ◽  
Dicobalt Octacarbonyl

AbstractA method to characterize open-cell nanoporous materials with atom probe tomography (APT) has been developed. For this, open-cell nanoporous gold with pore diameters of around 50 nm was used as a model system, and filled by electron beam-induced deposition (EBID) to obtain a compact material. Two different EBID precursors were successfully tested—dicobalt octacarbonyl [Co2(CO)8] and diiron nonacarbonyl [Fe2(CO)9]. Penetration and filling depth are sufficient for focused ion beam-based APT sample preparation. With this approach, stable APT analysis of the nanoporous material can be performed. Reconstruction reveals the composition of the deposited precursor and the nanoporous material, as well as chemical information of the interfaces between them. Thus, it is shown that, using an appropriate EBID process, local chemical information in three dimensions with sub-nanometer resolution can be obtained from nanoporous materials using APT.

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.

Quantitative Analysis of Precipitate Compositions in an Al-Li-Mg-Cu Alloy Using Atom Probe Tomography

2010 ◽  
Vol 654-656 ◽  
pp. 914-917 ◽  
Author(s):  
Xiang Yuan Xiong ◽  
Stavroula Moutsos ◽  
Russell King ◽  
Barry C. Muddle
Keyword(s):  
Quantitative Analysis ◽  
Aluminium Alloy ◽  
Atom Probe Tomography ◽  
Lithium Concentration ◽  
Stoichiometric Composition ◽  
Atom Probe ◽  
Field Evaporation ◽  
Experimental Conditions ◽  
3 Dimensional ◽  
Cu Alloy

The composition of  precipitates in aluminium alloy 8090 has been analysed using a 3 dimensional atom probe with fast data acquisition rates. The effects of experimental conditions for the quantitative atom probe analysis have been examined in detail. The results show that i) lithium is prone to preferential DC field evaporation at temperatures > 25K and with a pulse fraction < 20%; ii) the lithium concentration of  precipitates can vary from precipitate to precipitate, ranging from 19.1 to 25.3 at.%, and iii) the stoichiometric composition of the  phase can be obtained provided that the probing temperature is  25K and pulse fraction is  20%.

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