Hvem and Internal Oxidation Studies of Lithiated Nickel

1983 ◽  
Vol 27 ◽  
Author(s):  
K. Seshan ◽  
P. Baldo ◽  
H. Wiedersich

ABSTRACTPure, polycrystalline nickel samples were implanted with lithium to doses up to 5 × 1017 lithium ions per square centimeter, at a temperature of 500°C, such that the implantation damage would anneal. These samples were then prepared for electron microscopy and examined at 1 MeV, in the Argonne National Laboratory HVEM facility. It was observed that compared to pure nickel, the lithium implanted nickel showed a different radiation damage behaviour. A plausible explanation for the difference in behaviour is presented in this paper.The lithium implanted nickel, in the high dose samples, also showed an unusual form of precipitation. Electron microscopy revealed the precipitates to have truncated octahedral shapes with {111} planes for sides and {100} planes truncating the corners. They resemble voids and helium bubbles in nickel. The precipitates appear to be associated with dislocations. The lithium implanted nickel was internally oxidized in order to obtain evidence for the presence of lithium. Electron diffraction analysis of the internally oxidized lithiated nickel showed the presence of a topo-taxial compound being formed, with an ordered NaCl-structure. Possible interpretations of this diffraction pattern are discussed.

1987 ◽  
Vol 93 ◽  
Author(s):  
E. Gerritsen ◽  
H. J. Ligthart ◽  
T. E. G. Deenen

ABSTRACTPoly- and single crystalline copper was implanted with aluminium and nitrogen at doses ranging from 1016 to 5 × 1017 at/cm2 and energies of 170 keV. The corrosion resistance of the implanted surfaces was tested by exposure to an H25-containing atmosphere. The amount of copper sulphide formed was measured by chrono potentiometric reduction. The amount of corrosion products was markedly reduced (up to a factor 50) by high dose implantations of aluminium. The microstructure of the implanted copper was examined by Transmission Electron Microscopy of cross-sectioned specimens. A deep damage layer far exceeding the ion range was observed. XTEM-pictures of aluminium implanted copper single crystals of various orientations suggest a channeling mechanism for this deep damage layer. In situ annealing of the specimens in the TEM showed that most of the implantation damage is removed at 600°C except for an array of dislocations at the end of the damage range.


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.


1994 ◽  
Vol 373 ◽  
Author(s):  
N. Bordes ◽  
R.C. Ewing

AbstractBerlinite (AIPO4) is isostructural with α-quartz. Like α-quartz, berlinite undergoes a pressure-induced amorphization at 15 ±3 GPa; however, upon release of the pressure, unlike α-quartz which remains amorphous, berlinite returns to the original crystalline structure of the single crystal. Berlinite was irradiated with 1.5 MeV Kr+ at temperatures ranging from 20 to 600K. The onset of amorphization was examined by monitoring the electron diffraction pattern by in situ transmission electron microscopy (TEM) at the HVEM-Tandem Facility at Argonne National Laboratory. The berlinite was easily amorphized at 20K at a relatively low dose of 4x1013 ions/cm2 or 0.05 dpa (displacements per atom). The critical amorphization dose increases with the sample temperature. These experiments also showed that the focused electron beam can locally amorphize the berlinite. After these irradiations, berlinite remained amorphous. At 500 °C, berlinite began to recrystallize: small areas of crystalline material appear in the aperiodic matrix. These results suggest that pressure-induced amorphization and ion-beam induced amorphization, in the case of berlinite, are different processes that result in two different aperiodic structural states.


2005 ◽  
Vol 11 (5) ◽  
pp. 377-377
Author(s):  
Wayne King

The Ninth Frontiers of Electron Microscopy in Materials Science Conference (FEMMS 2003) was held October 5–10, 2003 at the Claremont Resort and Spa in Berkeley, CA. Major sponsors for this meeting included Lawrence Livermore National Laboratory, Argonne National Laboratory, Lawrence Berkeley National Laboratory, Brookhaven National Laboratory, Frederick Seitz Materials Research Laboratory, Oak Ridge National Laboratory, National Science Foundation, and University of California at Davis. Sponsors also included LEO Electron Microscopy Ltd. (Carl Zeiss SMT), E. A. Fischione, Inc., Gatan, Inc., Thermo NORAN (Thermo Electron Corp.), FEI Company, Hitachi-HHTA, JEOL USA, Inc., Seiko Instruments, and CEOS GmbH.


1996 ◽  
Vol 4 (8) ◽  
pp. 16-17
Author(s):  
David Henriks

An innovative technique has been developed which allows simultaneous cleaning of a sample and a specimen stage which minimizes and, in some cases eliminates, contamination of inorganic specimens analyzed via SEM.TEM, STEM and AEM.The technology involves subjecting the specimen and the specimen stage to a reactive plasma gas which efficiently removes a wide range of contaminants from critical surfaces. The procedure may be carried out prior to inserting the specimen and specimen stage into the EM via an externally produced accessory unit and can be extended for use on all types of electron microscopes where the sample and stage are loaded external to the instrument. Such an instrument was produced and implemented first by Dr. Nestor Zaluzec at Argonne National Laboratory. His system modified a commercially available pfasma etching system which included adapting it to accept a side entry holder.


2020 ◽  
Vol 7 (1) ◽  
Author(s):  
Maisaa N. Tawfeeq ◽  
Robert J. Klassen

Abstract Nickel and Helium ion implantation-induced hardening and microstructural evolution of X750 in the heat-treated (HT) and solution annealed (SA) conditions were investigated using nano-indentation hardness testing and electron microscopy (scanning electron microscopy (SEM) and transmission electron microscopy (TEM)). Irradiation crystal damage up to ψ = 5 dpa was invoked with Ni+ implantation while He+ implantation up to CHe = 5000 appm was performed on samples the HT and SA conditions. The X750 alloy displayed generally increasing hardness with increasing Ni+ implantation damage but a perturbation in the trend occurred when ψ ≤ 0.5 dpa, and the hardness dropped by about 30% and 2% for the HT and the SA samples, respectively. TEM analysis indicated that this softening was associated with disordering and dissolution of the γ′ strengthening phase. The hardening behavior observed at higher implantation damage (ψ = 1 dpa) resulted in reformation of Al/Ti-rich regions within the microstructure phase. The hardness of the X750 increased continuously with increasing implanted He+ up to CHe = 1000 appm. This was associated with the formation of helium bubbles as observed by TEM. Slight drop in hardness in the HT condition at CHe = 5000 appm indicated that high levels of He+ implantation destabilize the γ′ precipitates as was confirmed with TEM observed disappearance of γ′ super-lattice reflections.


1997 ◽  
Vol 481 ◽  
Author(s):  
A. T. Motta ◽  
A. Paesano ◽  
R. C. Birtcher ◽  
E. A. Ryan ◽  
M. E. Bruckmann ◽  
...  

ABSTRACTA detailed study has been conducted of the effect of Kr ion irradiation on phase formation in Zr-Fe metallic multilayers, using the Intermediate Voltage Electron Microscopy (IVEM) at Argonne National Laboratory. Metallic multilayers were prepared with different overall compositions (near 50–50 and Fe-rich), and with different wavelengths (repetition thicknesses). These samples were irradiated with 300 keV Kr ions at various temperatures to investigate the final products, as well as the kinetics of phase formation. For the shorter wavelength samples, the final product was in all cases an amorphous Zr-Fe phase, in combination with Fe, while specially for the larger wavelength samples, in the Fe-rich samples the intermetallic compounds ZrFe2 and Zr3Fe were formed in addition to the amorphous phase. The dose to full reaction decreases with temperature, and with wavelength in a manner consistent with a diffusion-controlled reaction.


Author(s):  
M. Isaacson ◽  
M.L. Collins ◽  
M. Listvan

Over the past five years it has become evident that radiation damage provides the fundamental limit to the study of blomolecular structure by electron microscopy. In some special cases structural determinations at very low doses can be achieved through superposition techniques to study periodic (Unwin & Henderson, 1975) and nonperiodic (Saxton & Frank, 1977) specimens. In addition, protection methods such as glucose embedding (Unwin & Henderson, 1975) and maintenance of specimen hydration at low temperatures (Taylor & Glaeser, 1976) have also shown promise. Despite these successes, the basic nature of radiation damage in the electron microscope is far from clear. In general we cannot predict exactly how different structures will behave during electron Irradiation at high dose rates. Moreover, with the rapid rise of analytical electron microscopy over the last few years, nvicroscopists are becoming concerned with questions of compositional as well as structural integrity. It is important to measure changes in elemental composition arising from atom migration in or loss from the specimen as a result of electron bombardment.


Author(s):  
N. D. Evans ◽  
M. K. Kundmann

Post-column energy-filtered transmission electron microscopy (EFTEM) is inherently challenging as it requires the researcher to setup, align, and control both the microscope and the energy-filter. The software behind an EFTEM system is therefore critical to efficient, day-to-day application of this technique. This is particularly the case in a multiple-user environment such as at the Shared Research Equipment (SHaRE) User Facility at Oak Ridge National Laboratory. Here, visiting researchers, who may oe unfamiliar with the details of EFTEM, need to accomplish as much as possible in a relatively short period of time.We describe here our work in extending the base software of a commercially available EFTEM system in order to automate and streamline particular EFTEM tasks. The EFTEM system used is a Philips CM30 fitted with a Gatan Imaging Filter (GIF). The base software supplied with this system consists primarily of two Macintosh programs and a collection of add-ons (plug-ins) which provide instrument control, imaging, and data analysis facilities needed to perform EFTEM.


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.


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