High resolution studies of the solid state amorphization reaction in the ZrCo system with the atom probe/field ion microscope

1994 ◽  
Vol 343 ◽  
Author(s):  
Susanne Schneider ◽  
Ralf Busch ◽  
Konrad Samwer

ABSTRACTThe atom probe/field ion microscope is introduced as a new powerful investigation device to study the early stages of the solid state amorphization reaction (SSAR). A bilayer of Zr and Co was condensed under UHV conditions on W wire tips and analyzed in a field ion microscope (FIM) combined with an atom probe (AP). The reaction of Co with Zr has been studied at room temperature. FIM pictures and AP analysis have shown that even at low temperatures an amorphous phase is formed at the Zr/Co interface and in the Zr grain boundaries. In these areas concentration profiles have been taken on a nanometer scale. Most likely, the extended solid solution of Co found in α- Zr grain boundaries causes the formation of the amorphous phase. Further, Rutherford backscattering spectrometry (RBS) suggests that even point defects and dislocations at the surface of an α- Zr single crystal are sufficient to initiate the SSAR between a polycrystalline Co layer vapour- deposited onto that single crystal.

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.


The measurement of low concentrations of elements segregated to or near grain boundaries with a spatial resolution of ca . 1 nm has recently become possible with the introduction of the imaging atom probe (i.a.p.). This development of the original atom probe field ion microscope uses a time-gated image intensifier as the detector of a time-of-flight mass spectrometer and displays an elemental map of ions desorbed from the surface of a field-ion specimen. The sensitivity of the analysis is uniform for both light (e.g. B, C, O) and heavy (e.g. Sn) elements, and concentrations down to 100 pg/g can be detected; accurate quantitative analyses are obtained by using the more conventional type of atom probe.


1994 ◽  
Vol 343 ◽  
Author(s):  
Ralf Busch ◽  
Frank Gaertner ◽  
Susanne Schneider ◽  
Rüdiger Bormann ◽  
Peter Haasen

ABSTRACTBased on atom probe field ion microscopy (AP/FIM) studies, electromotive force (EMF) measurements and CALPHAD calculations we discuss the earliest stage of the solid state amorphization reaction (SSAR) in Zr/Co-layers. The AP measurements show that two amorphous phases are formed at the Zr/Co interface from the early stages of the reaction. The metastable two phase field between these amorphous phases is shown by direct measurement of the chemical potential of Zr in amorphous co-sputtered ZrCo alloys by the EMF method. The comparison between the atom probe data and the CALPHAD calculation shows that the interfaces between the different layers are far away from metastable equilibrium in the beginning of the reaction. The amorphous phase formation at the Zr/Co interface and in the hcp-Zr grain boundary is preceded by a supersaturation of the hep ZrCo solid solution that transforms polymorphically into the amorphous state.


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):  
G. L. Kellogg ◽  
P. R. Schwoebel

Although no longer unique in its ability to resolve individual single atoms on surfaces, the field ion microscope remains a powerful tool for the quantitative characterization of atomic processes on single-crystal surfaces. Investigations of single-atom surface diffusion, adatom-adatom interactions, surface reconstructions, cluster nucleation and growth, and a variety of surface chemical reactions have provided new insights to the atomic nature of surfaces. Moreover, the ability to determine the chemical identity of selected atoms seen in the field ion microscope image by atom-probe mass spectroscopy has increased or even changed our understanding of solid-state-reaction processes such as ordering, clustering, precipitation and segregation in alloys. This presentation focuses on the operational principles of the field-ion microscope and atom-probe mass spectrometer and some very recent applications of the field ion microscope to the nucleation and growth of metal clusters on metal surfaces.The structure assumed by clusters of atoms on a single-crystal surface yields fundamental information on the adatom-adatom interactions important in crystal growth. It was discovered in previous investigations with the field ion microscope that, contrary to intuition, the initial structure of clusters of Pt, Pd, Ir and Ni atoms on W(110) is a linear chain oriented in the <111> direction of the substrate.


Author(s):  
Amanda K. Petford-Long ◽  
A. Cerezo ◽  
M.G. Hetherington

The fabrication of multilayer films (MLF) with layer thicknesses down to one monolayer has led to the development of materials with unique properties not found in bulk materials. The properties of interest depend critically on the structure and composition of the films, with the interfacial regions between the layers being of particular importance. There are a number of magnetic MLF systems based on Co, several of which have potential applications as perpendicular magnetic (e.g Co/Cr) or magneto-optic (e.g. Co/Pt) recording media. Of particular concern are the effects of parameters such as crystallographic texture and interface roughness, which are determined by the fabrication conditions, on magnetic properties and structure.In this study we have fabricated Co-based MLF by UHV thermal evaporation in the prechamber of an atom probe field-ion microscope (AP). The multilayers were deposited simultaneously onto cobalt field-ion specimens (for AP and position-sensitive atom probe (POSAP) microanalysis without exposure to atmosphere) and onto the flat (001) surface of oxidised silicon wafers (for subsequent study in cross-section using high-resolution electron microscopy (HREM) in a JEOL 4000EX. Deposi-tion was from W filaments loaded with material in the form of wire (Co, Fe, Ni, Pt and Au) or flakes (Cr). The base pressure in the chamber was around 8×10−8 torr during deposition with a typical deposition rate of 0.05 - 0.2nm/s.


1991 ◽  
Vol 232 ◽  
Author(s):  
M. K Miller ◽  
P. P. Camus ◽  
M. G. Hetherington

ABSTRACTThe atom probe field ion microscope has been used to characterize the morphology and determine the compositions of the iron-rich a and chromium-enriched α′ phases produced during isothermal and step cooled heat treatments in a Chromindur II ductile permanent magnet alloy. The good magnetic properties of this material are due to a combination of the composition of the two phases and the isolated nature and size of the ferromagnetic a phase. The morphology of the a phase is produced as a result of the shape of the miscibility gap and the step-cooled heat treatment and is distinctly different from that formed during isothermal heat treatments.


1995 ◽  
Vol 87-88 ◽  
pp. 279-283
Author(s):  
R.A. King ◽  
R.A.D. Mackenzie ◽  
G.D.W. Smith ◽  
N.A. Cade

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