Effets of surfaces on precipitate morphology in irradiated thin foils

Author(s):  
D.I. Potter ◽  
A. Taylor

Thermal aging of Ni-12.8 at. % A1 and Ni-12.7 at. % Si produces spatially homogeneous dispersions of cuboidal γ'-Ni3Al or Ni3Si precipitate particles arrayed in the Ni solid solution. We have used 3.5-MeV 58Ni+ ion irradiation to examine the effect of irradiation during precipitation on precipitate morphology and distribution. The nearness of free surfaces produced unusual morphologies in foils thinned prior to irradiation. These thin-foil effects will be important during in-situ investigations of precipitation in the HVEM. The thin foil results can be interpreted in terms of observations from bulk irradiations which are described first.Figure 1a is a dark field image of the γ' precipitate 5000 Å beneath the surface(∿1200 Å short of peak damage) of the Ni-Al alloy irradiated in bulk form. The inhomogeneous spatial distribution of γ' results from the presence of voids and dislocation loops which can be seen in the bright field image of the same area, Fig. 1b.

2014 ◽  
Vol 1712 ◽  
Author(s):  
Xiaoou. Yi ◽  
Michael L. Jenkins ◽  
Steve G. Roberts ◽  
Marquis A. Kirk

ABSTRACTIn our earlier work [1] microstructural evolution in tungsten under self-ion irradiation was investigated as a function of temperature and dose by in-situ 150 keV W+ ion irradiations on the IVEM-Tandem facility at Argonne National Laboratory (ANL). The present work focuses on the thermal stability of this damage. Thin foils of tungsten were irradiated at room temperature (R.T.) to fluences up to 1018 W+m-2 (∼ 1.0 dpa) and were then annealed in-situ for up to 120 min at temperatures between 300 and 800°C.We found that: (1) loops with Burgers vectors ½ <111> and <100> coexist during annealing; (2) <100> is not a stable loop configuration above 300°C and the fraction of such loops decreased with increasing temperature and/or time; (3) changes in loop populations during annealing were very sensitive to temperature, but less sensitive to time. The majority of changes occurred within 15 min, and were associated with the loss of small (1-2 nm) dislocation loops. The origin of these trends is discussed by considering defect mobility and the energetics of defect configurations predicted by previous DFT calculations [2].


1995 ◽  
Vol 398 ◽  
Author(s):  
Luciano Pagano ◽  
Arthur T. Motta ◽  
Robert C. Birtcher

ABSTRACTWe report here the results of a study conducted to examine the effect of Kr ion irradiation on bubble formation in Zr alloys. We used the HVEM/Tandem facility at Argonne National Laboratory to irradiate several Zr alloys, including Zircaloy-2 and Zircaloy-4, at temperatures from 300 to 800 C and to doses up to 2 × 1016ion.cm−2. Both in-situ irradiation of thin foils as well as irradiation of bulk samples with an ion implanter were used in this study. For the thin foil irradiations, a distribution of small bubbles in the range of 30-100 Å was found, at all temperatures with the exception of the Cr-rich Valloy where bubbles of 130 Å were found. The irradiation of bulk samples at high temperature (700–800 C) produced large faceted bubbles (up to 300 Å) after irradiation to 2 × 1016ion.cm−2. The results are examined in the context of existing models for bubble formation and growth in other metals.


Author(s):  
Prakash Rao

Image shifts in out-of-focus dark field images have been used in the past to determine, for example, epitaxial relationships in thin films. A recent extension of the use of dark field image shifts has been to out-of-focus images in conjunction with stereoviewing to produce an artificial stereo image effect. The technique, called through-focus dark field electron microscopy or 2-1/2D microscopy, basically involves obtaining two beam-tilted dark field images such that one is slightly over-focus and the other slightly under-focus, followed by examination of the two images through a conventional stereoviewer. The elevation differences so produced are usually unrelated to object positions in the thin foil and no specimen tilting is required.In order to produce this artificial stereo effect for the purpose of phase separation and identification, it is first necessary to select a region of the diffraction pattern containing more than just one discrete spot, with the objective aperture.


Author(s):  
J. R. Reed ◽  
D. J. Michel ◽  
P. R. Howell

The Al6Li3Cu (T2) phase, which exhibits five-fold or icosahedral symmetry, forms through solid state precipitation in dilute Al-Li-Cu alloys. Recent studies have reported that the T2 phase transforms either during TEM examination of thin foils or following ion-milling of thin foil specimens. Related studies have shown that T2 phase transforms to a microcrystalline array of the TB phase and a dilute aluminum solid solution during in-situ heating in the TEM. The purpose of this paper is to report results from an investigation of the influence of ion-milling on the stability of the T2 phase in dilute Al-Li-Cu alloy.The 3-mm diameter TEM disc specimens were prepared from a specially melted Al-2.5%Li-2.5%Cu alloy produced by conventional procedures. The TEM specimens were solution heat treated 1 h at 550°C and aged 1000 h at 190°C in air to develop the microstructure. The disc specimens were electropolished to achieve electron transparency using a 20:80 (vol. percent) nitric acid: methanol solution at -60°C.


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.


MRS Advances ◽  
2016 ◽  
Vol 1 (42) ◽  
pp. 2893-2899 ◽  
Author(s):  
R.W. Harrison ◽  
H. Amari ◽  
G. Greaves ◽  
J.A. Hinks ◽  
S.E. Donnelly

AbstractIn-situ ion irradiation and transmission electron microscopy has been used to examine the effects of the He appm to DPA ratio, temperature and dose on the damage structure of tungsten (W). Irradiations were performed with 15 or 60 keV He+ ions, achieving He-appm/displacements per atom (DPA) ratios of ∼40,000 and ∼2000, respectively, at temperatures between 500 and 1000°C to a dose of ∼3 DPA. A high number of small dislocation loops with sizes around 5–20 nm and a He bubble lattice were observed for both He-appm/DPA ratios at 500°C with a bubble size ∼1.5 nm. Using the g.b=0 criterion the loops were characterised as b = ±1/2<111> type. At 750°C bubbles do not form an ordered array and are larger in size compared to the irradiations at 500°C, with a diameter of ∼3 nm. Fewer dislocation loops were observed at this temperature and were also characterised to be b = ±1/2<111> type. At 1000°C, no dislocation loops were observed and bubbles grew as a function of fluence attributed to vacancy mobility being higher and vacancy clusters becoming mobile.


2017 ◽  
Vol 50 (4) ◽  
pp. 1028-1035 ◽  
Author(s):  
Hongbing Yu ◽  
Zhongwen Yao ◽  
Fei Long ◽  
Peyman Saidi ◽  
Mark R. Daymond

This study reportsin situobservations of the formation of the δ′-ZrO phase, occurring during the annealing of transmission electron microscopy (TEM) thin foils of both pure Zr and a Zr–Sn–Nb–Mo alloy at 973 K in a transmission electron microsope. The lattice parameters of δ′-ZrO were measured and determined to be similar to those of the ω-Zr phase. The orientation relationship between the δ′-ZrO and α-Zr phases has been identified as either {(11 \overline{2}0)}_{\rm ZrO}//{(0002)}_{\alpha} and {[0002]}_{\rm ZrO}//{[11 \overline{2}0]}_{\alpha} or {(\overline{1}011)}_{\rm ZrO}//{(0002)}_{\alpha} and {[01{\overline 1}1]_{{\rm{ZrO}}}}//{[11{\overline 2}0]_\alpha} depending on the orientation of the α grain relative to the TEM thin-foil normal. The nucleation and growth of δ′-ZrO were dynamically observed. This study suggests a new and convenient way to study oxidation mechanisms in Zr alloys and provides a deeper understanding of the properties of the newly reported δ′-ZrO. Since δ′-ZrO has a Zr sublattice which is identical to that of ω-Zr, the orientation relationships between the α and δ′-ZrO phases may also shed light on the orientation relations existing between α- and ω-Zr, and hence α- and ω-Ti.


1988 ◽  
Vol 100 ◽  
Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher ◽  
Lynn E. Rehn ◽  
Gerard L. Hofman

ABSTRACTUranium intermetallics are under consideration as possible low-enrichment reactor fuels. These materials divide into two classes with regard to dimensional stability during their service lifetime: those which suffer extreme dimensional growth and those which do not. It has been suggested that the rapid-swelling materials are those that become glassy under irradiation while the low-swelling materials are those that remain crystalline. The structural and dimensional stabilities of U3Si (depleted uranium) have been investigated as a function of temperature duning Kr irradiation by in situ. HVEM observations. Below 550 K, this material becomes glassy during 1.0 MeV Kr irradiation. Prolonged irradiation at 475 K also leads to rapid darkening of the TEM bright field image of the specimen, growth of the initial perforation at rates which far exceed those due to sputtering, and formation of additional thin areas and holes. Irradiation at 615 K does not result in observable image darkening or rapid growth of the initial perforation. After 2×1020 Kr m-2, the crystalline material irradiated at 615 K is stabilized against subsequent ion-irradiation-induced amorphization and growth at 475 K. Similarly, after 2×1020 Kr m-2 at 475 K, the glassy phase persists at 620 K under additional Kr irradiation, and the rapid growth continues. The mechanism of the irradiation-induced growth of the glassy material does not involve gas precipitation but rather may involve deformation by viscous flow assisted by the defects generated during irradiation.


1998 ◽  
Vol 539 ◽  
Author(s):  
J.K. Heuer ◽  
N.Q. Lam ◽  
P.R. Okamoto ◽  
J.F. Stubbins

AbstractRecent studies have shown that high stress concentrations at moving crack tips in the intermetallic compound NiTi can induce a crystalline-to-amorphous (C-A) transformation of the crack tip region. This stress-induced C-A transformation has a temperature dependence and crystallization behavior similar to those of ion irradiation-induced C-A transformation of NiTi. The present study examines if these similarities between stress- and irradiation-induced amorphization hold true for two other intermetallic compounds, CuTi and Ni3Ti. In situ straining was performed in an intermediate-voltage transmission electron microscope. The presence or absence of an amorphous phase was determined by dark field imaging and selected area diffraction of crack tip regions. Crack tips in both CuTi and Ni3Ti were found to remain crystalline upon fracture. The observed absence of stress-induced amorphization in Ni3Ti is consistent with its known absence during irradiation, but the absence in CuTi differs from its known irradiation-induced amorphization behavior. Reasons for the similarity and difference are discussed.


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