Characterization of Internal Interfaces by Atom Probe Field Ion Microscopy

1992 ◽  
Vol 295 ◽  
Author(s):  
M. K. Miller ◽  
Raman Jayaram

AbstractThe near atomic spatial resolution of the atom probe field ion microscope permits the elemental characterization of internal interfaces, grain boundaries and surfaces to be performed in a wide variety of materials. Information such as the orientation relationship between grains, topology of the interface, and the coherency of small precipitates with the surrounding matrix may be obtained from field ion microscopy. Details of the solute segregation may be obtained at the plane of the interface and as a function of distance from the interface for all elements simultaneously from atom probe compositional analysis. The capabilities and limitations of the atom probe technique in the characterization of internal interfaces is illustrated with examples of grain boundaries and interphase interfaces in a wide range of materials including intermetallics, model alloys, and commercial steels.

Author(s):  
K. F. Russell ◽  
M. K. Miller

The atom probe field ion microscope (APFIM) is well suited to the characterization of the fine scale features and defects that are formed in materials due to exposure to neutron irradiation. However, in order for the technique to be effective, suitable specimens are required. Atom probe field ion microscopy specimens are in the form of ultrasharp needles that are usually produced by a series of mechanical and chemical or electrochemical methods. These needles have a typical end radius of approximately 10 to 50 nm and a taper angle of between 1 and 5. The small dimensions mean that the specimens are extremely fragile and difficult to handle and do not easily lend themselves to remote operations in a hot cell. The small size and mass of the APFIM specimen has the advantage that the amount of material required is minimal.A concept in working with irradiated materials is to keep exposure to the operator "as low as reasonably achievable" (ALARA).


MRS Bulletin ◽  
1994 ◽  
Vol 19 (7) ◽  
pp. 27-34 ◽  
Author(s):  
M.K. Miller ◽  
G.D.W. Smith

The atom probe field ion microscope is the most powerful and direct method for the analysis of materials at the atomic level. Since analyses are performed by collecting atoms one at a time from a small volume, it is possible to conduct fundamental characterization of materials at this level. The atom probe technique is applicable to a wide range of materials since its only restriction is that the material under analysis must possess at least some limited electrical conductance. Therefore, since its introduction in 1968, the atom probe field ion microscope has been used in many diverse applications in most branches of materials science. Many of the applications have exploited its high spatial resolution capabilities to perform microstructural characterizations of features such as grain boundaries and other interfaces and ultrafine scale precipitation that are not possible with other microanaly tical techniques. This article briefly outlines some of the capabilities and applications of the atom probe. The details of the atom probe technique are described elsewhere.The power of the atom probe may be demonstrated by its ability to see and identify a single atom, which is particularly useful in characterizing solute segregation to grain boundaries or other interfaces. An example of a brightly-imaging solute atom at a grain boundary in a nickel aluminide is shown in Figure 1. In order to conclusively determine its identity, its image is aligned with the probe aperture in the center of the imaging screen and then the selected atom is carefully removed by field evaporation and analyzed in the time-of-flight mass spectrometer. This and many other bright spots in this material were shown to be boron atoms. This example also illustrates the light element analytical capability of the atom probe. In fact, the atom probe may to used to analyze all elements in the periodic table and has had applications ranging from characterizing the distribution of implanted hydrogen to phase transformations in uranium alloys.


1989 ◽  
Vol 4 (6) ◽  
pp. 1549-1559 ◽  
Author(s):  
Tien T. Tsong ◽  
Chong-lin Chen ◽  
Jiang Liu

Our recent applications of the atom-probe field ion microscope to the study of physics and chemistry of materials at the atomic level are summarized. The materials applicability of field ion microscopy has recently been extended to silicon, silicide, graphite, high Tc superconductors, and other materials. Atom-probe field ion microscopy has been used for atomic layer by atomic layer chemical analysis of surfaces in alloy and impurity segregations, for analyzing the compositional changes across metal-semiconductor interfaces, and for studying formation of cluster ions in laser stimulated field desorption. The energetics of atoms in solids and on surfaces can be studied by a direct kinetic energy analysis of field desorbed ions using a high resolution pulsed-laser time-of-flight atom-probe and by other field ion microscope measurements. The site specific binding energy of surface atoms can be measured at low temperature, where the atomic structure of the surface is still perfectly defined, to an accuracy of about 0.1 to 0.3 eV.


2020 ◽  
Vol 26 (2) ◽  
pp. 247-257 ◽  
Author(s):  
Benjamin M. Jenkins ◽  
Frédéric Danoix ◽  
Mohamed Gouné ◽  
Paul A.J. Bagot ◽  
Zirong Peng ◽  
...  

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.


Author(s):  
M.G. Burke ◽  
M.K. Miller

In the development of advanced alloys for power system applications, the primary emphasis is placed on attaining specific mechanical properties with resistance to environmental attack. An important part of alloy development is the detailed characterization of the microstructure, because it is the composition, size and morphology of the microstructural features that define the mechanical properties of the material. The good mechanical properties of Ni-base superalloys are a result of the formation of fine coherent precipitates. In addition, other coarser phases may form which can degrade the properties of the alloys. Analytical electron microscopy (AEM) provides important information concerning the type and distribution of the phases in the alloys, but quantitative microchemical analysis of the ultra-fine precipitates is not readily obtainable with conventional AEM techniques. The high spatial resolution of the atom probe field-ion microscope (APFIM) makes this technique ideally suited to the analysis of the ultra-fine precipitates and surrounding matrix. The analysis of the matrix is particularly important in predicting the subsequent ageing response of the alloy, as previously shown in a detailed AEM/APFIM examination of Alloy 718. In this paper, a combined AEM/APFIM study of precipitation in Alloy X-750 is presented.


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