scholarly journals In Situ Ion Beam Research In Argonne's Intermediate Voltage Electron Microscope

1996 ◽  
Vol 439 ◽  
Author(s):  
Charles W. Allen ◽  
Edward A. Ryan

AbstractSince Fall 1995, a state-of-the-art intermediate voltage electron microscope (IVEM) has been operational in the HVEM-Tandem Facility with in situ ion irradiation capabilities similar to those of the HVEM of the Facility. A 300 kV Hitachi H-9000NAR is interfaced to the two ion accelerators of the Facility, with a demonstrated point-topoint spatial resolution for imaging of 0.25 nm with the ion beamline attached to the microscope. The IVEM incorporates a Faraday cup system for ion dosimetry with measurement aperture 6.5 cm from the TEM specimen, which was described in Symposium A of the 1995 MRS Fall Meeting. The IVEM is now employed for a variety of in situ ion beam studies ranging from low dose ion damage experiments with GaAs, in which damage zones individual displacement cascades are observed, to implantation studies in metals, in which irradiation-induced noble gas precipitate mobility is studied in real time. In this presentation, the new instrumentation and its specifications will be described briefly, several basic concepts relating to in situ experiments in transmission electron microscopes will be summarized and examples of in situ experiments will be presented which exploit the experimental capabilities of this new user facility instrumentation.

1995 ◽  
Vol 396 ◽  
Author(s):  
Charles W. Allen ◽  
Loren L. Funk ◽  
Edward A. Ryan

AbstractDuring 1995, a state-of-the-art intermediate voltage electron microscope (IVEM) has been installed in the HVEM-Tandem Facility with in situ ion irradiation capabilities similar to those of the HVEM. A 300 kV Hitachi H-9000NAR has been interfaced to the two ion accelerators of the Facility, with a spatial resolution for imaging which is nearly an order of magnitude better than that for the 1.2 MV HVEM which dates from the early 1970s. The HVEM remains heavily utilized for electron- and ion irradiation-related materials studies, nevertheless, especially those for which less demanding microscopy is adequate. The capabilities and limitations of this IVEM and HVEM are compared. Both the HVEM and IVEM are part of the DOE funded User Facility and therefore are available to the scientific community for materials studies, free of charge for non-proprietary research.


1991 ◽  
Vol 235 ◽  
Author(s):  
Charles W. Allen

ABSTRACTMotivated at least initially by materials needs for nuclear reactor development, extensive irradiation effects studies employing transmission electron microscopes (TEM) have been performed for several decades, involving irradiation-induced and irradiation-enhanced microstructural changes, including phase transformations such as precipitation, dissolution, crystallization, amorphization, and order-disorder phenomena. From the introduction of commercial high voltage electron microscopes (HVEM) in the mid-1960s, studies of electron irradiation effects have constituted a major aspect of HVEM application in materials science. For irradiation effects studies two additional developments have had particularly significant impact; (1) the development of TEM specimen holders in which specimen temperature can be controlled in the range 10–2200 K and (2) the interfacing of ion accelerators which allows in situ TEM studies of irradiation effects and the ion beam modification of materials within this broad temperature range. This paper treats several aspects of in situ studies of electron and ion beam-induced and enhanced phase changes and presents two case studies involving in situ experiments performed in an HVEM to illustrate the strategies of such an approach of the materials research of irradiation effects.


Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher

The uranium silicides, including U3Si, are under study as candidate low enrichment nuclear fuels. Ion beam simulations of the in-reactor behavior of such materials are performed because a similar damage structure can be produced in hours by energetic heavy ions which requires years in actual reactor tests. This contribution treats one aspect of the microstructural behavior of U3Si under high energy electron irradiation and low dose energetic heavy ion irradiation and is based on in situ experiments, performed at the HVEM-Tandem User Facility at Argonne National Laboratory. This Facility interfaces a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter to a 1.2 MeV AEI high voltage electron microscope, which allows a wide variety of in situ ion beam experiments to be performed with simultaneous irradiation and electron microscopy or diffraction.At elevated temperatures, U3Si exhibits the ordered AuCu3 structure. On cooling below 1058 K, the intermetallic transforms, evidently martensitically, to a body-centered tetragonal structure (alternatively, the structure may be described as face-centered tetragonal, which would be fcc except for a 1 pet tetragonal distortion). Mechanical twinning accompanies the transformation; however, diferences between electron diffraction patterns from twinned and non-twinned martensite plates could not be distinguished.


Author(s):  
R. C. Birtcher ◽  
L. M. Wang ◽  
C. W. Allen ◽  
R. C. Ewing

We present here results of in situ TEM diffraction observations of the response of U3Si and U3Si2 when subjected to 1 MeV electron irradiation or to 1.5 MeV Kr ion irradiation, and observations of damage occuring in natural zirconolite. High energy electron irradiation or energetic heavy ion irradiation were performed in situ at the HVEM-Tandem User Facility at Argonne National Laboratory. In this Facility, a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter have been interfaced to a 1.2 MeV AEI high voltage electron microscope. This allows a wide variety of in situ experiments to be performed with simultaneous ion irradiation and conventional transmission electron microscopy. During the electron irradiation, the electron beam was focused to a diameter of about 2 μ.m at the specimen thin area. The ion beam was approximately 2 mm in diameter and was uniform over the entire specimen. With the specimen mounted in a heating holder, the temperature increase indicated by the furnace thermocouple during the ion irradiation was typically 8 °K.


1988 ◽  
Vol 100 ◽  
Author(s):  
Fu-Rong Ding ◽  
P. R. Okamoto ◽  
L. E. Rehn

ABSTRACTAu/Zr bilayer films with inert-gas markers were produced by low energy (< 4 keV) implantation. Mass transport was measured during ion-beam mixing with 1 MeV Kr at several temperatures between 330 and 540K. Two distinct regimes of apparent Arrhenius behavior were found with activation enthalpies of 0.06 and 0.9 eV in the temperature range 330–440K and 460–540K, respectively. Microstructural changes during ion-beam mixing were studied in situ, in a high voltage electron microscope. Heterogeneous nucleation of an amorphous phase was observed during mixing. The results are compared with similar studies reported previously in Ni/Zr bilayer specimens.


Author(s):  
K. Furuya ◽  
M. Osaki ◽  
S. Hagiwara ◽  
T. Saito

The ultra high voltage transmission electron microscope (UHV-TEM) having an acceleration voltage of 1000 kV or more has been used for the observation of atomic structure of materials because of its high resolution approaching to 0.1 nm. Few effort has been done to develop an analytical UHV-TEM with energy dispersive x-ray spectroscope (EDS) for in-situ experiments such as ion irradiation, because high density of hard x-ray accompanied with primary electrons is supposed to prevent to measure the characteristic x-ray from the specimen. However, the observation of the heterostructures and interfaces requires analytical capability of determining the local chemical composition compatible with high resolution electron microscopy. This paper describes about a new analytical UHV-TEM (AHV-TEM) equipped with EDS and energy filtered imaging system and its application to Ni silicide thin film.The AHV-TEM in this study is based on JEM-ARM1000 with a side entry goniometer. Figure 1 shows the comparison of calculated CTF and optical diffractogram of amorphous Ge taken near Scherzer defocus with E=1000 keV, Cs=2.6 mm, Cc=3.4 mm and Qi=0.3 mrad.


2010 ◽  
Vol 1265 ◽  
Author(s):  
Karl Whittle ◽  
Mark Blackford ◽  
Robert Aughterson ◽  
Katherine L Smith ◽  
Gregory R Lumpkin ◽  
...  

AbstractThin crystals of La2O3, La2/3TiO3, La2TiO5, and La2Ti2O7 have been irradiated in situ using 1 MeV Kr2+ ions in the Intermediate Voltage Electron Microscope-Tandem User Facility (IVEM-Tandem), at the Argonne National Laboratory (ANL). We observed that La2O3 remained crystalline to a fluence greater than 3.1 × 1016 ions cm-2 at a temperature of 50 K. The four binary oxide compounds in the two systems were observed through the crystalline-amorphous transition as a function of ion fluence and temperature. Results from the ion irradiations give critical temperatures for amorphisation (Tc) of 840 K for La2Ti2O7, 865 K for La2/3TiO3, and 1027 K for La2TiO5. The Tc values observed in this study, together with previous data for TiO2, are discussed with reference to the phase diagrams for La2O3-TiO2 systems and the different local environments within the crystal structures. Results suggest an observable inverse correlation between Tc and melting temperature (Tm) in the two systems.


Author(s):  
C. W. Allen ◽  
E. A. Ryan ◽  
S. T. Ockers

Established in 1981, the High Voltage Electron Microscope-Tandem Ion Accelerator Facility (HVEM-Tandem) is a user-oriented resource for materials research. It is located at Argonne National Laboratory about 20 miles south of O'Hare International Airport near Chicago. The Facility consists of a modified Kratos/AEI HVEM with accelerating voltages ranging continuously from 0.1-1.2 MeV, interfaced to a 2 MV tandem and a 0.65 MV ion implanter-type accelerator. This combination of instruments offers capability, unique in the western hemisphere, for a wide range of in Situ experiments involving ion irradiation and ion implantation with simultaneous microscopy. During 1987 approximately 75% of microscope time was devoted to this type of experiment (Fig. 1) including studies of solid state phase transformations, such as amorphization, radiation damage and defect structures and the implantation of noble gas and metal ions.In situ experiments of various types account for nearly 90% of usage of the HVEM. In addition to the radiation effects studies, this includes experiments performed in the microscope involving deformation, annealing and environmental effects.


Author(s):  
Charles W. Allen

When thin polycrystalline films of Au, Cu and various other materials are subjected to energetic ion irradiation, the average grain size increases even at cryogenic temperatures. As is the case with many ion beam processes, this phenomenon of ion irradiation induced grain growth exhibits only a very mild temperature dependence. This contribution is based on in situ experiments, performed at the HVEM-Tandem User Facility at Argonne National Laboratory. This Facility interfaces a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter to a 1.2 MV AEI high voltage electron microscope, which allows a wide variety of in situ ion beam experiments to be performed with simultaneous irradiation and electron microscopy or diffraction. A series of in situ ion and/or electron irradiation experiments is being performed at the HVEM-Tandem Facility at Argonne which have shown clearly for fine grained Au films that two mechanisms for growth are operative for the ion beam case: grain boundary migration as in normal thermal grain growth and grain coalescence which is similar in appearance to recrystallization by subgrain coalescence. Especially in the case of Au for which ion-induced growth is relatively rapid, such in situ experiments also demonstrate the importance of dislocation activity which is a consequence of the collision cascade damage associated with ion irradiation. Existing theories for irradiation-induced grain growth assume that growth occurs by boundary migration and that only point defects generated at grain boundaries are responsible for the growth phenomenon.


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