Ion Beam Irradiation of Lanthanum Compounds in the Series La2O3-TiO2

2010 ◽  
Vol 1265 ◽  
Author(s):  
Karl Whittle ◽  
Mark Blackford ◽  
Robert Aughterson ◽  
Katherine L Smith ◽  
Gregory R Lumpkin ◽  
...  
Keyword(s):  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Inverse Correlation ◽  
Critical Temperatures ◽  
Voltage Electron ◽  
Local Environments ◽  
Two Systems ◽  
User Facility

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.

In Situ Radiation Damage Studies of Ca3Zr2FeAlSiO12 and Ca3Hf2FeAlSiO12

2008 ◽  
Vol 1124 ◽  
Author(s):  
Karl R Whittle ◽  
Mark Blackford ◽  
Gregory R Lumpkin ◽  
Katherine L Smith ◽  
Nestor J Zaluzec
Keyword(s):  
Nuclear Waste ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Voltage Electron ◽  
Significant Difference ◽  
User Facility ◽  
High Level Nuclear Waste ◽  
Nuclear Waste Immobilization ◽  
High Level

AbstractGarnets, A3B2C3O12, are considered to be potential host phases for the immobilization of high-level nuclear waste as they can accommodate a number of elements of interest, including Zr, Ti and Fe. The naturally occurring garnet, kimzeyite, Ca3(Zr,Ti)2(Si,Al,Fe)3O12, can contain ˜30wt% Zr. An understanding of the radiation tolerance of these materials is crucial to their potential use in nuclear waste immobilization. In this study two synthetic analogues of kimzeyite of composition Ca3Zr2FeAlSiO12 and Ca3Hf2FeAlSiO12 were monitored in situ during irradiation with 1.0 MeV Kr ions using the intermediate voltage electron microscope-Tandem User Facility (IVEM) at Argonne National Laboratory. The structure of these materials was previously determined by neutron diffraction and 57Fe Mössbauer spectroscopy. Ca3Zr2FeAlSiO12 and Ca3Hf2FeAlSiO12 have very similar structural properties with cubic Ia3d symmetry, the only significant difference being the presence of Zr and Hf, respectively, on the 6 coordinated B sites.

Electron and ion irradiation-induced dissolution of mechanical twins in the intermetalic U3Si: An in situ HVEM study

1989 ◽  
Vol 47 ◽  
pp. 652-653
Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher
Keyword(s):  
Elevated Temperatures ◽  
Ion Irradiation ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Heavy Ion ◽  
High Energy ◽  
Mechanical Twinning ◽  
In Situ Experiments

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.

Ion Irradiation of Ternary Pyrochlores

2008 ◽  
Vol 1122 ◽  
Author(s):  
Karl R. Whittle ◽  
Katherine L. Smith ◽  
Mark G. Blackford ◽  
Simon A.T. Redfern ◽  
Elizabeth J. Harvey ◽  
...  
Keyword(s):  
Ion Irradiation ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Structural Disorder ◽  
Critical Temperatures ◽  
High Doses

AbstractSynthetic pyrochlore samples Y2Ti2-xSnxO7 (x=0.4, 0.8, 1.2, 1.6), Nd2Zr2O7, Nd2Zr1.2Ti0.8O7, and La1.6Y0.4Hf2O7, were irradiated in-situ using the IVEM-TANDEM microscope facility at the Argonne National Laboratory. The critical temperatures for amorphisation have revealed a dramatic increase in tolerance with increasing Sn content for the Y2Ti2-xSnxO7 series. This change has also found to be linear with increasing Sn content. Nd2Zr1.2Ti0.8O7 and La1.6Y0.4Hf2O7 were both found to amorphise, while Nd2Zr2O7 was found to be stable to high doses (2.5×10^15 ions cm-2). The observed results are presented with respect to previously published results for irradiation stability predictions and structural disorder.

New Instrumentation in Argonne's Hvem-Tandem Facility: Expanded Capability for in Situ Ion Beam Studies+

1995 ◽  
Vol 396 ◽  
Author(s):  
Charles W. Allen ◽  
Loren L. Funk ◽  
Edward A. Ryan
Keyword(s):  
Scientific Community ◽  
State Of The Art ◽  
Ion Irradiation ◽  
Ion Beam ◽  
Voltage Electron ◽  
User Facility ◽  
Order Of Magnitude ◽  
New Instrumentation ◽  
Better Than

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.

Amorphization Kinetics of Zr (Cr,Fe)2 Under Ion Irradiation

1992 ◽  
Vol 279 ◽  
Author(s):  
A. T. Motta ◽  
L. M. Howe ◽  
P. R. Okamoto
Keyword(s):  
Neutron Irradiation ◽  
Ion Irradiation ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Matrix Interface ◽  
Thin Foils ◽  
Intermetallic Precipitates ◽  
Kinetics Of

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.

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
Keyword(s):  
Electron Microscope ◽  
Ion Irradiation ◽  
Noble Gas ◽  
Ion Beam ◽  
Voltage Electron ◽  
In Situ Experiments ◽  
User Facility ◽  
New Instrumentation ◽  
Electron Microscopes

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.

Radiation-induced disordering and amorphization—An in situ HVEM study of uranium silicide with comparison to natural processes in zirconolite

1990 ◽  
Vol 48 (4) ◽  
pp. 534-535
Author(s):  
R. C. Birtcher ◽  
L. M. Wang ◽  
C. W. Allen ◽  
R. C. Ewing
Keyword(s):  
Electron Irradiation ◽  
Ion Irradiation ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Heavy Ion ◽  
High Energy ◽  
In Situ Tem ◽  
In Situ Experiments

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.

Characterization of Collision Cascade Damage in Ca2La8(SiO4)6O2 by Hrtem

1994 ◽  
Vol 373 ◽  
Author(s):  
L.M. Wang ◽  
W.J. Webert
Keyword(s):  
Elevated Temperatures ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Sample Surface ◽  
Thermal Recovery ◽  
Collision Cascade ◽  
Cascade Damage

AbstractCa2La8(SiO4)6O2 thin crystals become amorphous under ion beam irradiation. The ion dose required for complete amorphization of the thin crystal (critical amorphization dose, Dc) increased with the increasing irradiation temperature and decreased with ion mass at elevated temperatures. Samples irradiated with 1-1.5 MeV Ar+, Kr+ and Xe+ ions to doses much lower than Dc, in the temperature range from 20 to 498 K were used for a detailed HRTEM investigation to study the amorphization process. The residual collision cascade damage after irradiation appeared as nanometer scale amorphous domains. The images of these domains are extremely sensitive to the sample thickness. Small domains of cascade size were found only at the very thin edge of the sample. In thicker regions, amorphous domains appear after higher doses as the result of cascade overlap in projection. At higher temperatures, the observed amorphous domains are smaller indicating thermal recovery at the amorphous/crystalline interface. The amorphous domains are also larger in size after irradiation with ions of higher mass at a fixed ion dose. These results are consistent with the Dc-temperature curves determined by in situ TEM with the HVEM-Tandem Facility at Argonne National Laboratory. The width of the amorphous rim along the edge of the specimen grew with increasing ion dose suggesting that amorphization also proceeds from the sample surface. Images of the collision cascade damage were compared to the cascade sizes calculated with the TRIM code. Some digitally acquired HRTEM images of the cascade damage were processed to reveal more detailed information.

Ion-Beam Amortization of Ca2La2(SiO4)6O2 Single Crystals

1992 ◽  
Vol 279 ◽  
Author(s):  
William J. Weber ◽  
Lu-Min Wang
Keyword(s):  
Electron Microscopy ◽  
Single Crystals ◽  
Structural Changes ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Annealing Process ◽  
Recoil Energy ◽  
Transmission Electron

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.

scholarly journals Ion-Beam Mixing and Solid-State Reaction in Zr-Fe Multilayers

1996 ◽  
Vol 439 ◽  
Author(s):  
A. Paesano ◽  
A. T. Motta ◽  
R. C. Birtcher ◽  
E. A. Ryan ◽  
S. R. Teixeira ◽  
...  
Keyword(s):  
Solid State ◽  
Amorphous Phase ◽  
Solid State Reaction ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Reaction Products ◽  
Phase Selection ◽  
Voltage Electron ◽  
Multilayered Thin Films

AbstractVapor-deposited Zr-Fe multilayered thin films with various wavelengths and of overall composition either 50% Fe or Fe-rich up to 57 % Fe were either irradiated with 300 keV Kr ions at temperatures from 25K to 623 K to fluences up to 2 × 1016 cm−2, or simply annealed at 773K in-situ in the Intermediate Voltage Electron Microscope at Argonne National Laboratory. Under irradiation, the final reaction product is the amorphous phase in all cases studied, but the dose to amorphization depends on the temperature and on the wavelength. In the purely thermal case (annealing at 773 K), the 50–50 composition produces the amorphous phase but for the Fe-rich multilayers the reaction products depend on the multilayer wavelength. For small wavelength, the amorphous phase is still formed, but at large wavelength the Zr-Fe crystalline intermetallic compounds appear. These results are discussed in terms of existing models of irradiation kinetics and phase selection during solid state reaction.

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