Atom Probe Field Ion Microscopy and High Resolution Electron Microscopy: two complementary methods for atomic scale characterisation

Author(s):  
F. Danoix ◽  
T. Gloriant ◽  
T. Epicier ◽  
F. Vurpillot ◽  
W. Lefebvre
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.


1998 ◽  
Vol 4 (S2) ◽  
pp. 108-109
Author(s):  
K. Hono ◽  
D. H. Ping ◽  
M. Ohnuma

Atom probe field ion microscopy is the most suitable technique for determining local chemical composition changes during nanocrystallization processes of amorphous alloys. In this talk, we report atom probe field ion microscopy (APFIM) and high resolution electron microscopy (HREM) studies on nanocrystallization processes in Fe-Si-B-Nb-Cu soft magnet and Fe-Nd-B-Co-Ga exchange spring magnet.Fe or Co based alloys with nanocrystalline microstructure show excellent permeability because the net magnetocrystalline anisotropy is significantly reduced when the grain size becomes smaller than the ferromagnetic exchange length. Fe-Si-B-Nb-Cu alloy is the pioneering nanocrystalline soft magnetic material invented by Yoshizawa et al. in 1988 [1]. Our previous works [2,3] reported evidence for clustering of Cu prior to the onset of the crystallization reaction. However, in the previous studies, it was not confirmed that these Cu clusters work as heterogeneous nucleation sites for a-Fe primary crystals.


1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.


1989 ◽  
Vol 159 ◽  
Author(s):  
A. Catana ◽  
M. Heintze ◽  
P.E. Schmid ◽  
P. Stadelmann

ABSTRACTHigh Resolution Electron Microscopy (HREM) was used to study microstructural changes related to the CoSi/Si-CoSi/CoSi2/Si-CoSi2/Si transformations. CoSi is found to grow epitaxially on Si with [111]Si // [111]CoSi and < 110 >Si // < 112 >CoSi. Two CoSi non-equivalent orientations (rotated by 180° around the substrate normal) can occur in this plane. They can be clearly distinguished by HRTEM on cross-sections ( electron beam along [110]Si). At about 500°C CoSi transforms to CoSi2. Experimental results show that the type B orientation relationship satisfying [110]Si // [112]CoSi is preserved after the initial stage of CoSi2 formation. At this stage an epitaxial CoSi/CoSi2/Si(111) system is obtained. The atomic scale investigation of the CoSi2/Si interface shows that a 7-fold coordination of the cobalt atoms is observed in both type A and type B epitaxies.


1990 ◽  
Vol 202 ◽  
Author(s):  
A. Catana ◽  
P.E. Schmid

ABSTRACTHigh Resolution Electron Microscopy (HREM) and image calculations are combined to study microstructural changes related to the CoSi/Si-CoSi/CoSi2/Si-CoSi2/Si transformations. The samples are prepared by UHV e-beam evaporation of Co layers (2 nm) followed by annealing at 300°C or 400°C. Cross-sectional observations at an atomic scale show that the silicidation of Co at the lower temperature yields epitaxial CoSi/Si domains such that [111]Si // [111]CoSi and <110>Si // <112>CoSi. At about 400°C CoSi2 nucleates at the CoSi/Si interface. During the early stages of this chemical reaction, an epitaxial CoSi/CoSi2/Si system is observed. The predominant orientation is such that (021) CoSi planes are parallel to (220) CoSi2 planes, the CoSi2/Si interface being of type B. The growth of CoSi2 is shown to proceed at the expense of both CoSi and Si.


MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 26-31 ◽  
Author(s):  
Robert Sinclair

Processing has always been a key component in the development of new materials. Basic scientific understanding of the reactions and transformations that occur has obvious importance in guiding progress. Invaluable insight can be provided by observing the changes during processing, especially at high magnification by in situ microscopy. Now that this can be achieved at the atomic level by using high-resolution electron microscopy (HREM), atomic behavior can be seen directly. Accordingly, many deductions concerning reactions in materials at the atomic scale are possible.The purpose of this article is to illustrate the level reached by in situ HREM. The essential procedure is to form a high-resolution image of a standard transmission electron microscope (TEM) sample and then to alter the structure by some means in a controlled manner, such as by heating. Continual recording on videotape allows subsequent detailed analysis of the behavior, even on a frame-by-frame (1/30 second) basis. The most obvious advantage is to follow the atomic rearrangements directly in real time. However, in addition, by continuous recording no stages in a reaction are missed, which can often occur in a series of conventional ex situ annealed samples because of the limited number of samples that can realistically be examined by HREM. One can be sure that the same reaction, in the same area, is being studied. Furthermore, by changing the temperature systematically, extremely precise kinetic measurements can be made (e.g., for activation energies and kinetic laws) and the whole extent of a material transformation can be investigated in one sample, something that would take months of work if studied conventionally. The information provided by in situ HREM is often unique and so it can become an important technique for fundamental materials investigations.


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