The evolution of the microstructure of 600 Mev proton irradiated materials

Author(s):  
R. Gotthardt ◽  
A. Horsewell ◽  
F. Paschoud ◽  
S. Proennecke ◽  
M. Victoria

Fusion reactor materials will be damaged by an intense field of energetic neutrons. There is no neutron source of sufficient intensity at these energies available at present, so the material properties are being correlated with those obtained in irradiation with other irradiation sorces. Irradiation with 600 MeV protons produces both displacement damage and impurities due to nuclear reactions. Helium and hydrogen are produced as gaseous impurities. Other metallic impurities are also created . The main elements of the microstructure observed after irradiation in the PIREX facility, are described in the following paragraphs.A. Defect clusters at low irradiation doses: In specimens irradiated to very low doses (1021-1024 protons.m-2), so that there is no superimposition of contrast, small defect clusters have been observed by the weak beam technique. Detailed analysis of the visible contrast (>0.5 nm diameter) revealed the presence of stacking fault tetrahedra, dislocation loops and a certain number of unidentified clusters . Typical results in Cu and Au are shown in Fig. 1.

Author(s):  
J. E. O'Neal ◽  
S. M. L. Sastry ◽  
J. W. Davis

The radiation-induced defect structure and nonequilibrium phase precipitation were studied in T1-6A1-4V (an alpha-beta titanium alloy), irradiated at 450 ± 30°C in row VII of the EBR-II to a fluence of 3.0 × 1021 neutrons/cm2 (En > 0.1 MeV). The Irradiation-induced defect microstructures were examined using bright-field, conventional dark-field, and weak-beam dark-field techniques. The nature of dislocations and dislocation loops was determined by standard-contrast experiments under two-beam conditions, and the small defect clusters were identified using the line-of-contrast criterion and black-white vector orientation criterion.


Author(s):  
Robert C. Rau ◽  
Robert L. Ladd ◽  
John Moteff

Transmission electron microscopy has been used to study the microstructure of vanadium irradiated at reactor ambient temperature (∼ 70°C) to a fast (E > 1 MeV) neutron fluence of 5 x 1019 n/cm2. Observations were made of the as-irradiated material, and after one-hour vacuum annealing at various temperatures ranging from 330°C to 1175°C.In the as-irradiated condition, shown in Fig. 1, a very high density of small defect clusters was present. These clusters appeared as black dots averaging approximately 25-50 Å in diameter, and were estimated to be present in quantities of 1016 to 1017 per cm3. Post-irradiation annealing caused the clusters to increase in average size and decrease in number, as shown in Figs. 2 and 3, until after the highest temperature anneal, 1175°C, the cluster density was legs than 1014 per cm3 and the average cluster size was approximately 500Å. After annealing at temperatures of 510°C or above, many of the clusters were seen to be resolvable as dislocation loops. Tilting experiments indicated that these loops were probably interstitial in nature.


1998 ◽  
Vol 540 ◽  
Author(s):  
M. A. Kirk ◽  
M. L. Jenkins ◽  
H. Fukushima

AbstractA low-temperature in situ ion-irradiation and annealing experiment has been performed by TEM in copper. Most defect clusters which persisted through an anneal to 120 K showed no size changes within the resolution (0.5 nm) of a new weak-beam sizing technique. Of 55 defects measured under a range of weakly diffracting conditions, 7 showed measurable size decreases while 3 showed size increases. We argue that these clusters are likely to be of vacancy and interstitial nature, respectively. Also on annealing to 120 K a fraction of about 25% of the clusters formed by irradiation with 600 kV Cu+ ions at 20 K disappeared, while a similar number of clusters appeared in different locations.


Crystals ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 257 ◽  
Author(s):  
Bennett C. Larson

Deviations of crystal diffraction line profiles from those predicted by the dynamical theory of diffraction for perfect crystals provide a window into the microscopic distributions of defects within non-perfect crystals. This overview provides a perspective on key theoretical, computational, and experimental developments associated with the analysis of diffraction line profiles for crystals containing statistical distributions of point defect clusters, e.g., dislocation loops, precipitates, and stacking fault tetrahedra. Pivotal theoretical developments beginning in the 1940s are recalled and discussed in terms of their impact on the direction of theoretical and experimental investigations of lattice defects in the 1960s, the 1970s, and beyond, as both experimental and computational capabilities advanced. The evolution of experimental measurements and analysis techniques, as stimulated by theoretical and computational progress in understanding the distortion fields surrounding defect clusters, is discussed. In particular, consideration is given to determining dislocation loop densities and separate size distributions for vacancy and interstitial type loops, and to the internal strain and size distributions for coherent precipitates.


1993 ◽  
Vol 316 ◽  
Author(s):  
Rebecca X. Ai ◽  
Nicole Bordes ◽  
Elizabeth A. Cooper ◽  
Kurt E. Sickafus ◽  
Rodney C. Ewing ◽  
...  

ABSTRACTThis study examines the influence of microstructural defects on irradiation damage accumulation in the oxide spinel. Single crystals of the compound MgAl2O4 with surface normal [111] were irradiated under cryogenic temperature (100°K) either with 50 keV Ne ions (fluence 5.0 × 1012/cm2), 400 keV Ne ions (fluence 6.7 × 1013cm2) or successively with 400 keV Ne ions followed by 50 keV Ne ions. The projected range of 50 keV Ne ions in spinel is ~50 nm (“shallow”) while the projected range of 400 keV Ne ions is ~ 500 nm (“deep”). Transmission electron microscopy (TEM) was used to examine dislocation loops/ defect clusters formed by the implantation process. Measurements of the dislocation loop size were made using weak-beam imaging technique on cross-sectional TEM ion-implanted specimens. Defect clusters were observed in both deep and shallow implanted specimens, while dislocation loops were observed in the shallow implanted sample that was previously irradiated by 400 keV Ne ions. Cluster size was seen to increase for shallow implants in crystals irradiated with a deep implant (size ~8.5 nm) as compared to crystals treated only to a shallow implant (size ~3.1 nm).


Author(s):  
Robert C. Rau ◽  
John Moteff

Transmission electron microscopy has been used to study the thermal annealing of radiation induced defect clusters in polycrystalline tungsten. Specimens were taken from cylindrical tensile bars which had been irradiated to a fast (E > 1 MeV) neutron fluence of 4.2 × 1019 n/cm2 at 70°C, annealed for one hour at various temperatures in argon, and tensile tested at 240°C in helium. Foils from both the unstressed button heads and the reduced areas near the fracture were examined.Figure 1 shows typical microstructures in button head foils. In the unannealed condition, Fig. 1(a), a dispersion of fine dot clusters was present. Annealing at 435°C, Fig. 1(b), produced an apparent slight decrease in cluster concentration, but annealing at 740°C, Fig. 1(C), resulted in a noticeable densification of the clusters. Finally, annealing at 900°C and 1040°C, Figs. 1(d) and (e), caused a definite decrease in cluster concentration and led to the formation of resolvable dislocation loops.


Author(s):  
T. Y. Tan ◽  
W. K. Tice

In studying ion implanted semiconductors and fast neutron irradiated metals, the need for characterizing small dislocation loops having diameters of a few hundred angstrom units usually arises. The weak beam imaging method is a powerful technique for analyzing these loops. Because of the large reduction in stacking fault (SF) fringe spacing at large sg, this method allows for a rapid determination of whether the loop is faulted, and, hence, whether it is a perfect or a Frank partial loop. This method was first used by Bicknell to image small faulted loops in boron implanted silicon. He explained the fringe spacing by kinematical theory, i.e., ≃l/(Sg) in the fault fringe in depth oscillation. The fault image contrast formation mechanism is, however, really more complicated.


Author(s):  
C. B. Carter ◽  
J. Rose ◽  
D. G. Ast

The hot-pressing technique which has been successfully used to manufacture twist boundaries in silicon has now been used to form tilt boundaries in this material. In the present study, weak-beam imaging, lattice-fringe imaging and electron diffraction techniques have been combined to identify different features of the interface structure. The weak-beam technique gives an overall picture of the geometry of the boundary and in particular allows steps in the plane of the boundary which are normal to the dislocation lines to be identified. It also allows pockets of amorphous SiO2 remaining in the interface to be recognized. The lattice-fringe imaging technique allows the boundary plane parallel to the dislocation to be identified. Finally the electron diffraction technique allows the periodic structure of the boundary to be evaluated over a large area - this is particularly valuable when the dislocations are closely spaced - and can also provide information on the structural width of the interface.


Author(s):  
J. M. Oblak ◽  
B. H. Kear

The “weak-beam” and systematic many-beam techniques are the currently available methods for resolution of closely spaced dislocations or other inhomogeneities imaged through strain contrast. The former is a dark field technique and image intensities are usually very weak. The latter is a bright field technique, but generally use of a high voltage instrument is required. In what follows a bright field method for obtaining enhanced resolution of partial dislocations at 100 KV accelerating potential will be described.A brief discussion of an application will first be given. A study of intermediate temperature creep processes in commercial nickel-base alloys strengthened by the Ll2 Ni3 Al γ precipitate has suggested that partial dislocations such as those labelled 1 and 2 in Fig. 1(a) are in reality composed of two closely spaced a/6 <112> Shockley partials. Stacking fault contrast, when present, tends to obscure resolution of the partials; thus, conditions for resolution must be chosen such that the phase shift at the fault is 0 or a multiple of 2π.


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