The formation and recrystallization of amorphous zones produced in GaAS by ion irradiation

Author(s):  
M. W. Bench ◽  
I. M. Robertson ◽  
M. A. Kirk

Transmission electron microscopy experiments have been performed to investigate the lattice damage created by heavy-ion bombardments in GaAs. These experiments were undertaken to provide additional insight into the mechanisms by which individual amorphous zones and eventually amorphous layers are created. To understand these mechanisms, the structure of the defects created as a function of material, irradiating ion, dose, dose rate, and implantation tenperature have been studied using TEM. Also, the recovery of the crystalline structure by annealing has been investigated.These experiments were performed at the High-Voltage Electron Microscope - Ion Accelerator Facility at Argonne National Laboratory. This facility consists of an HVEM which has been interfaced with two ion accelerators. This coupling, plus the availability of several specimen stages permits ion irradiations to be performed in the specimen chamber of the microscope at controlled temperatures from 10 to 1000 K.

1988 ◽  
Vol 100 ◽  
Author(s):  
M. W. Bench ◽  
I. M. Robertson ◽  
M. A. Kirk

ABSTRACTTransmission electron microscopy experiments have been performed to investigate the lattice damage created by heavy-ion bombardments in GaAs. These experiments have been performed in situ by using the HVEN - Ion Accelerator Facility at Argonne National Laboratory. The ion bcorbardments (50 keV Ar+ and Kr+) and the microscopy have been carried out at temperatures rangrin from 30 to 300 K. Ion fluences ranged from 2 × 1011 to 5 × 1013 ions cm−2.Direct-inpact amorphization is observed to occur in both n-type and semi-insulating GaAs irradiated to low ion doses at 30 K and room temperature. The probability of forming a visible defect is higher for low temperature irradiations than for room temperature irradiations. The amorphous zones formed at low temperature are stable to temperatures above 250 K. Post implantation annealing is seen to occur at room temperature for all samples irradiated to low doses until eventually all visible damage disappears.


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

Although it was initially thought that irradiation could not further damage an amorphous material, an anomalous ion-induced morphological instability on the surface of amorphous Ge has been reported previously by several authors. In this study, the structural and morphological changes of Ge were monitored during 1.5 MeV Kr ion irradiation by in situ TEM to obtain insight into the damage evolution in ion-irradiated Ge.The in situ study was performed on the HVEM-Tandem Accelerator Facility at Argonne National Laboratory. The facility consists of a modified Kratos/AEI EM7 high voltage electron microscope (HVEM) and a 2 MV tandem ion accelerator. The samples were jet-polished polycrystalline Ge (99.99999 at. % pure) TEM discs with grain size > 5 μm in dimension. The Kr ion irradiation was carried out at room temperature, and the electron energy of the HVEM was 300 kV. According to a TRIM computer simulation, over 99% of the Kr ions penetrate through the electron transparent areas of the Ge sample, and a dose of 1×1015 Kr/cm2 created an average of ∽4 displacements per atom and an average Kr concentration of ∽12 appm in the observation region of the sample.


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.


1994 ◽  
Vol 353 ◽  
Author(s):  
T. J. White ◽  
R. C. Ewing ◽  
L. M. Wang ◽  
J. S. Forrester ◽  
C. Montross

AbstractA transmission electron microscope investigation was made of zirconolites and perovskites irradiated to amorphization with 1 MeV krypton ions using the HVEM-Tandem Facility at Argonne National Laboratory. Three specimens were examined - a prototype zirconolite CaZrTi2O7, a gadolinium doped zirconolite Ca0.75Gd0.50Zr0.75Ti2O7and a uranium doped zirconolite Ca0.75U0.50Zr0.75Ti2O7. The critical amorphization dose Dc was determined at several temperatures between 20K to 675K. Dc was inversely proportional with temperature. For example, pure zirconolite requiring 10x the dose for amorphization at 475K compared with gadolinium zirconolite. Using an Arrhenius plot, the activation energy Ea for annealing in these compounds was found to be 0.129 eV and 0.067 eV respectively. The greater ease of amorphization for the gadolinium sample is probably a reflection of this element’s large cross section for interaction with heavy ions. Uranium zirconolite was very susceptible to damage and amorphised under 4 keV argon ions during the preparation of microscope specimens. In each sample, zirconolite coexisted with minor perovskite, reduced rutile (Magneli phases) and zirconia. These phases were more resistant to ion irradiation than zirconolite. Even for high gadolinium loadings, perovskite (Ca0.8Gd0.2TiO3) was 3-4 times more stable to ion irradiation than the surrounding zirconolite crystals.


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.


1997 ◽  
Vol 481 ◽  
Author(s):  
R. Devanathan ◽  
W. J. Weber ◽  
L. A. Boatner

ABSTRACTZircon (ZrSiO4) is an actinide host phase in vitreous ceramic nuclear waste forms and a potential host phase for the disposition of excess weapons plutonium. In the present work, the effects of 800 and 900 keV electron, and 1 MeV Ne+ irradiations on the structure of single crystals of ZrSiO4 have been investigated. The microstructural evolution during the irradiations was studied in situ using a high-voltage electron microscope interfaced to an ion accelerator at Argonne National Laboratory. The results indicate that electron irradiation at 15 K cannot amorphize ZrSiO4 even at fluences an order of magnitude higher than that required for amorphization by 1.5 MeV Kr + ions. However, the material is readily amorphized by I MeV Ne+ irradiation at 15 K. The temperature dependence of this amorphization is discussed in light of previous studies of radiation Zdamage in ZrSiO4.


1997 ◽  
Vol 3 (S2) ◽  
pp. 773-774
Author(s):  
Katherine L. Smith ◽  
Nestor J. Zaluzec ◽  
Gregory R. Lumpkin

Zirconolite (CaZrTi2O7) is the major host phase for actinides in Synroc, a promising waste form for the immobilisation of high-level radioactive waste. The effect of radiation damage on the structure and durability of zirconolite are important to predictive modelling of zirconolite's behaviour in the repository environment and risk assessment.In this study, radiation damage effects in zirconolite were investigated by irradiating samples with 1.5 MeV Kr+ ions using the HVEM-Tandem at Argonne National Laboratory (ANL) and energy loss electron spectroscopy (EELS). The HVEM-Tandem consists of a modified AEI high votage transmission electron microscope interfaced to to a 2 MV tandem ion accelerator. EELS spectra were collected using a Philips 420 TEM, operated at 120 kV, fitted with a Gatan Model 607 Serial EELS. EELS data were recorded at resolutions of ˜1.0 eV and at a dispersion of about ˜0.25 eV.Selected area diffraction patterns (SADs) of individual grains of various zirconolites were monitored as a function of dose to establish the critical dose for aniorphisation (Dc).


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