In Situ Hvem Studies of Electron-Beam-Driven Composition Changes in Thin Film Alloys: Displacement-Rate Gradient Effects

1984 ◽  
Vol 41 ◽  
Author(s):  
P. R. Okamoto ◽  
N. Q. Lam

AbstractIn situ high-voltage electron microscopy (HVEM) observations have shown that the highly-focused electron beams normally employed for HVEM irradiation experiments can cause large chemical composition changes in the irradiated zone of thin film alloys during elevated temperature irradiations. The driving force for the process comes primarily from the radial gradients in displacement rates generated by the beam. Hence, the rate of change in composition exhibits a strong dependence not only on the temperature and beam intensity, but also on the spatial characteristics of the beam profile. This dependence on beam shape and size poses previously unrecognized problems, particularly for HVEM studies of the effects of dose-rate on radiation-induced phenomena that are sensitive to alloy composition. Moreover, composition changes driven by radial gradients in the displacement- rate occur at increasingly rapid rates as the beam diameter is reduced. Hence, at higher voltages, beam-induced composition changes occurring during analysis may become a serious problem, even at relatively low temperatures, for microchemical analysis techniques, such as EDX and EELS, which employ far smaller diameter electron beams than those used for irradiation purposes in the HVEM.

Author(s):  
J. A. Pollock ◽  
M. Martone ◽  
T. Deerinck ◽  
M. H. Ellisman

Localization of specific proteins in cells by both light and electron microscopy has been facilitate by the availability of antibodies that recognize unique features of these proteins. High resolution localization studies conducted over the last 25 years have allowed biologists to study the synthesis, translocation and ultimate functional sites for many important classes of proteins. Recently, recombinant DNA techniques in molecular biology have allowed the production of specific probes for localization of nucleic acids by “in situ” hybridization. The availability of these probes potentially opens a new set of questions to experimental investigation regarding the subcellular distribution of specific DNA's and RNA's. Nucleic acids have a much lower “copy number” per cell than a typical protein, ranging from one copy to perhaps several thousand. Therefore, sensitive, high resolution techniques are required. There are several reasons why Intermediate Voltage Electron Microscopy (IVEM) and High Voltage Electron Microscopy (HVEM) are most useful for localization of nucleic acids in situ.


Author(s):  
J N Chapman ◽  
W A P Nicholson

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.


Author(s):  
K. Barmak

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.


Author(s):  
M. Park ◽  
S.J. Krause ◽  
S.R. Wilson

Cu alloying in Al interconnection lines on semiconductor chips improves their resistance to electromigration and hillock growth. Excess Cu in Al can result in the formation of Cu-rich Al2Cu (θ) precipitates. These precipitates can significantly increase corrosion susceptibility due to the galvanic action between the θ-phase and the adjacent Cu-depleted matrix. The size and distribution of the θ-phase are also closely related to the film susceptibility to electromigration voiding. Thus, an important issue is the precipitation phenomena which occur during thermal device processing steps. In bulk alloys, it was found that the θ precipitates can grow via the grain boundary “collector plate mechanism” at rates far greater than allowed by volume diffusion. In a thin film, however, one might expect that the growth rate of a θ precipitate might be altered by interfacial diffusion. In this work, we report on the growth (lengthening) kinetics of the θ-phase in Al-Cu thin films as examined by in-situ isothermal aging in transmission electron microscopy (TEM).


Author(s):  
E. Holzäpfel ◽  
F. Phillipp ◽  
M. Wilkens

During in-situ radiation damage experiments aiming on the investigation of vacancy-migration properties interstitial-type dislocation loops are used as probes monitoring the development of the point defect concentrations. The temperature dependence of the loop-growth rate v is analyzed in terms of reaction-rate theory yielding information on the vacancy migration enthalpy. The relation between v and the point-defect production rate P provides a critical test of such a treatment since it is sensitive to the defect reactions which are dominant. If mutual recombination of vacancies and interstitials is the dominant reaction, vαP0.5 holds. If, however, annihilation of the defects at unsaturable sinks determines the concentrations, a linear relationship vαP is expected.Detailed studies in pure bcc-metals yielded vαPx with 0.7≾×≾1.0 showing that besides recombination of vacancies and interstitials annihilation at sinks plays an important role in the concentration development which has properly to be incorporated into the rate equations.


2002 ◽  
Vol 725 ◽  
Author(s):  
S.B. Phelan ◽  
B.S. O'Connell ◽  
G. Farrell ◽  
G. Chambers ◽  
H.J. Byrne

AbstractThe current voltage characteristics of C60 thin film sandwich structures fabricated by vacuum deposition on indium tin oxide (ITO) with an aluminium top electrode are presented and discussed. A strongly non-linear behavior and a sharp increase in the device conductivity was observed at relatively low voltages (∼2V), at both room and low temperatures (20K). At room temperature the system is seen to collapse, and in situ Raman measurements indicate a solid state reduction of the fullerene thin film to form a polymeric state. The high conductivity state was seen to be stable at elevated voltages and low temperatures. This state is seen to be reversible with the application of high voltages. At these high voltages the C60 film was seen to sporadically emit white light at randomly localized points analogous to the much documented Electroluminescence in single crystals.


2000 ◽  
Vol 650 ◽  
Author(s):  
Lance L. Snead ◽  
Martin Balden

ABSTRACTDensification and crystallization kinetics of bulk SiC amorphized by neutron irradiation is studied. The temperature of crystallization onset of this highly pure, fully amorphous bulk SiC was found to be between 875-885°C and crystallization is nearly complete by 950°C. In-situ TEM imaging confirms the onset of crystallization, though thin-film effects apparently alter the kinetics of crystallization above this temperature. It requires >1125°C for complete crystallization of the TEM foil. Annealing at temperatures between the irradiation and crystallization onset temperature is seen to cause significant densification attributed to a relaxation, or reordering, of the as-amorphized structure.


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