In sito Ion Beam Analysis of Radiation Damage Kinetics in MgTiO3 Single Crystals at 170-470 K

1995 ◽  
Vol 396 ◽  
Author(s):  
Ning Yu ◽  
Jeremy N. Mitchell ◽  
Kurt E. Sickafus ◽  
Michael Nastasi

AbstractRadiation damage kinetics in synthetic MgTiO3 (geikielite) single crystals have been studied using the in situ ion beam facility at Los Alamos National Laboratory. The geikielite samples were irradiated at temperatures of 170, 300, and 470 K with 400 keV xenon ions and the radiation damage was sequentially measured with Rutherford backscattering using a 2 MeV He ion beam along a channeling direction. Threshold doses of 1 and 5×1015 Xe/cm2 were determined for the crystalline-to-amorphous transformation induced by Xe ion irradiation at 170 and 300 K, respectively. However, geikielite retained its crystallinity up to a dose of 2.5x1016 Xe/cm2 at the irradiation temperature of 470 K. This study has shown that MgTiO3, which has a corundum derivative structure, is another radiation resistant material that has the potential for use in radiation environments.

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.


1992 ◽  
Vol 279 ◽  
Author(s):  
A. T. Motta ◽  
L. M. Howe ◽  
P. R. Okamoto

ABSTRACTThin foils of Zircaloy-4 were irradiated with 350 KeV 40Ar ions in the dual ion beam/HVEM facility at Argonne National Laboratory at 300 – 650 K. The irradiation-induced araorphization of the intermetallic precipitates Zr (Cr, Fe)2 and Zr2 (Ni, Fe) was studied in situ. For Zr (Cr,Fe)2 precipitates the dose-to-amorphization was found to increase exponentially with temperature, with a critical temperature of about 650 K. The amorphization morphology was shown to be homogeneous, with no preferential site for nucleation, in contrast to neutron-irradiation amorphization which started at the precipitate-matrix interface. For Zr2 (Ni,Fe) precipitates it was found that amorphization occurred at 550 K and 600 K, whereas in neutron irradiation no amorphization has been observed at those temperatures. The results are discussed in the context of the previous experimental results of neutron and electron irradiation and likely amorphization mechanisms are proposed.


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.


Author(s):  
Ning Yu ◽  
Timothy E. Levine ◽  
Kurt E. Sickafus ◽  
Michael Nastasi ◽  
Jeremy N. Mitchell ◽  
...  

1995 ◽  
Vol 10 (4) ◽  
pp. 981-985 ◽  
Author(s):  
N. Bordes ◽  
L.M. Wang ◽  
R.C. Ewing ◽  
K.E. Sickafus

Ion-irradiation induces amorphization in many intermetallics and ceramics, but spinel (MgAl2O4) is considered a “radiation resistant” ceramic. Spinel was irradiated with 1.5 MeV Kr+ at 20 K and observed in situ by transmission electron microscopy (TEM). The spinel remained crystalline to a high dose of 1 × 1016 ions/cm2, without any evidence of amorphization. Another spinel was preimplanted with Ne (400 keV and 50 keV). The microstructure revealed a still crystalline material with 8 nm interstitial loops. After irradiation with 1.5 MeV Kr+ (20 K), amorphization, a result of cation disordering, initiated at a dose of 1.7 × 1015 ions/cm2. At a dose of 1 × 1016 ions/cm2, the spinel was partially amorphous and the remaining crystalline domains disordered. These results show that spinel can be disordered and that amorphization can be triggered by the introduction of stable defects, followed by ion irradiation at low temperature.


1992 ◽  
Vol 279 ◽  
Author(s):  
William J. Weber ◽  
Lu-Min Wang

ABSTRACTSingle crystals of Ca2La8(SiO4)6O2 were irradiated with 1.5 MeV Xe+, 1.5 MeV Kr+, 1.0 MeV Ar+ and 0.8 MeV Ne+ ions to investigate the effects of recoil-energy spectrum, temperature, and crystallographic orientation on irradiation-induced amorphization. The irradiations were carried out using the HVEM-Tandem Facility at Argonne National Laboratory. The structural changes and the ion fluence for complete amorphization in the electron transparent thickness of the specimens were determined by in situ transmission electron microscopy. The displacement dose determined for complete amorphization was approximately 0.6 dpa for the Xe+, Kr+, and Ar+ ion irradiations but increased to 1.4 dpa for the Ne+ ion irradiations, which may reflect an effect of lower recoil energies. The ion fluence for complete amorphization increased exponentially with temperature over the range from 25 to 400°C. Amorphization was not observed at 500°C. The activation energy associated with this simultaneous annealing process was estimated to be 0.13 eV, and the critical amorphization temperature was estimated to be 438°C for the 1.5 MeV Kr+ irradiations.


1992 ◽  
Vol 268 ◽  
Author(s):  
L.M. Wang ◽  
A.Y. Wu ◽  
R.C. Ewing

ABSTRACTPLZT 9/65/35 single crystals were irradiated with 1.5 MeV krypton ions at 25–450°C in the HVEM-Tandem Facility at Argonne National Laboratory. In-situ TEM was performed during irradiation in order to determine the critical amorphization dose. At room temperature, the material was completely amorphized after a dose of only 1.9×1014 ions/cm2, less than one fifth of the critical amorphization dose for silicon (1×1015 ions/cm2). The critical amorphization dose for the PLZT material increased with increasing irradiation temperature. At 450°C, amorphization was not observed after a dose of 1.1×10 15ions/cm2.


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.


2002 ◽  
Vol 713 ◽  
Author(s):  
Jie Lian ◽  
Sergey V. Yudintsev ◽  
Sergey V. Stefanovsky ◽  
Olga I. Kirjanova ◽  
Rodney C. Ewing

ABSTRACTMurataite A4B2C7O22-x, where A = Na+, Ca2+, REE3+, An3+/4+; B = Mn2+/3+, Zn2+; C = Ti4+, Fe3+, Al3+; 0≤x≤1, is an isometric, derivative of the fluorite-structure. Murataite is potentially suitable as a phase for the immobilization of rare earth (REE) and actinide elements (An). Murataite structures with three-(3C), five-(5C), and eight-fold (8C) multiples of the fluorite unit cell parameters have been identified. Radiation-induced amorphization of murataite has been investigated by 1 MeV Kr+ ion irradiation of three ceramic samples produced by melting in a resistive furnace and a cold crucible at 1400-1600 °C. The 1 MeV Kr+ ion irradiations were performed at room temperature using IVEM-Tandem Facility at Argonne National Laboratory. Radiation damage was observed by in-situ TEM. Initially, the irradiation caused disordering of the murataite structure. Murataite was rendered fully amorphous at a dose of (1.7∼1.9)Á1018 ion/m2. The pyrochlore structure phase (2C) is more radiation resistant to ion irradiation-induced amorphization than the murataite structure. Combining results on murataite with those pyrochlore and fluorite, a generally increasing trend in the susceptibility to ion beam damage is found in the fluorite-related structures as a function of the increasing multiples of the fluorite unit cells.


1993 ◽  
Vol 321 ◽  
Author(s):  
W. J. Weber ◽  
N. J. Hess ◽  
L. M. Wang

ABSTRACTSingle crystals of Ca2La8(SiO4)6O2, with 1% Nd substituted for La, were irradiated with 0.8 MeV Ne+ and 1.5 MeV Kr+ ions over the temperature range from 15 K to 773 K. The irradiations were carried out using the HVEM-Tandem Facility at Argonne National Laboratory. The structural changes and the ion fluence for complete amorphization were determined by in situ transmission electron Microscopy. The ion fluence for complete amorphization increased with temperature in two stages associated with defect annealing processes. The critical temperature for amorphization increased from -360 K for 0.8 MeV Ne+ to -710 K for 1.5 MeV Kr+. During in situ annealing studies, irradiation-enhanced recrystallization was observed at 923 K. Spatially-resolved fluorescence spectra of the Nd ion excited with 488.0 nm laser excitation showed marked line-broadening toward the center of the amorphous regions. Initial Measurements indicate the subtle shifts of the 9I9/2 groundstate energy levels can be measured by pumping directly into the excited state 4F3/2 Manifold suggesting that the line broadening observed originates from a distribution of geometrically distorted Nd sites.


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