In situ Transmission Electron Microscopy Investigation of Radiation Effects

2005 ◽  
Vol 20 (7) ◽  
pp. 1654-1683 ◽  
Author(s):  
R.C. Birtcher ◽  
M.A. Kirk ◽  
K. Furuya ◽  
G.R. Lumpkin ◽  
M-O. Ruault
Keyword(s):  
Radiation Effects ◽  
Ion Irradiation ◽  
Ion Beam ◽  
Ex Situ ◽  
In Situ Observation ◽  
Dislocation Loops ◽  
Transmission Electron ◽  
Microscopy Investigation ◽  
Ion Impact

In situ observation is of great value in the study of radiation damage utilizing electron or ion irradiation. We summarize the facilities and give examples of work found around the world. In situ observations of irradiation behavior have fallen into two broad classes. One class consists of long-term irradiation, with observations of microstructural evolution as a function of the radiation dose in which the advantage of in situ observation has been the maintenance of specimen position, orientation, and temperature. A second class has involved the recording of individual damage events in situations in which subsequent evolution would render the correct interpretation of ex situ observations impossible. In this review, examples of the first class of observation include ion-beam amorphization, damage accumulation, plastic flow, implant precipitation, precipitate evolution under irradiation, and damage recovery by thermal annealing. Examples of the second class of observation include single isolated ion impacts that produce defects in the form of dislocation loops, amorphous zones, or surface craters, and single ion impact-sputtering events. Experiments in both classes of observations attempt to reveal the kinetics underlying damage production, accumulation, and evolution.

A comparison of radiation effects in crystalline ABO4-type phosphates and silicates

2000 ◽  
Vol 64 (2) ◽  
pp. 185-194 ◽  
Author(s):  
A. Meldrum ◽  
L. A. Boatner ◽  
R. C. Ewing
Keyword(s):  
Damage Accumulation ◽  
Radiation Effects ◽  
Ion Irradiation ◽  
Ion Beam ◽  
Chemical Compositions ◽  
Transmission Electron ◽  
Host Materials ◽  
High Level Nuclear Waste ◽  
High Level

AbstractThe effects of ion irradiation in the ABO4-type compounds were compared by performing experiments on four materials that include the most common crystal structures (monazite vs. zircon) and chemical compositions (phosphates vs. silicates) for these phases. Pure synthetic single crystals of ZrSiO4, monoclinic ThSiO4, LaPO4 and ScPO4 were irradiated using 800 keV Kr+ ions. Radiation damage accumulation was monitored as a function of temperature in situ in a transmission electron microscope. The activation energies for recrystallization during irradiation were calculated to be 3.1–3.3 eV for the orthosilicates but only 1.0–1.5 eV for the isostructural orthophosphates. For the ion-beam-irradiated samples, the critical temperature, above which the recrystallization processes are faster than damage accumulation and amorphization cannot be induced, is >700°C for ZrSiO4 but it is only 35°C for LaPO4. At temperatures above 600°C, zircon decomposed during irradiation into its component oxides (i.e. crystalline ZrO2 plus amorphous SiO2). The data are evaluated with respect to the proposed use of the orthophosphates and orthosilicates as host materials for the stabilization and disposal of high-level nuclear waste. The results show that zircon with 10 wt.% Pu would have to be maintained at temperatures in excess of 300°C in order to prevent it from becoming completely amorphous. In contrast, a similar analysis for the orthophosphates implies that monazite-based waste forms would not become amorphous or undergo a phase decomposition.

scholarly journals Direct Characterization of the Relation between the Mechanical Response and Microstructure Evolution in Aluminum by Transmission Electron Microscopy In Situ Straining

Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1431
Author(s):  
Seiichiro Ii ◽  
Takero Enami ◽  
Takahito Ohmura ◽  
Sadahiro Tsurekawa
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Elastic Behavior ◽  
Annealed Specimen ◽  
Displacement Curve ◽  
Dislocation Loops ◽  
Transmission Electron ◽  
Stress Drops

Transmission electron microscopy in situ straining experiments of Al single crystals with different initial lattice defect densities have been performed. The as-focused ion beam (FIB)-processed pillar sample contained a high density of prismatic dislocation loops with the <111> Burgers vector, while the post-annealed specimen had an almost defect-free microstructure. In both specimens, plastic deformation occurred with repetitive stress drops (∆σ). The stress drops were accompanied by certain dislocation motions, suggesting the dislocation avalanche phenomenon. ∆σ for the as-FIB Al pillar sample was smaller than that for the post-annealed Al sample. This can be considered to be because of the interaction of gliding dislocations with immobile prismatic dislocation loops introduced by the FIB. The reloading process after stress reduction was dominated by elastic behavior because the slope of the load–displacement curve for reloading was close to the Young’s modulus of Al. Microplasticity was observed during the load-recovery process, suggesting that microyielding and a dislocation avalanche repeatedly occurred, leading to intermittent plasticity as an elementary step of macroplastic deformation.

scholarly journals Ion-Irradiation-Induced Amorphization Of Cadmium Niobate Pyrochlore

2000 ◽  
Vol 650 ◽  
Author(s):  
A. Meldrum ◽  
K. Beaty ◽  
L. A. Boatner ◽  
C. W. White
Keyword(s):  
Electron Microscope ◽  
Ambient Temperature ◽  
Transmission Electron Microscope ◽  
Room Temperature ◽  
Ion Irradiation ◽  
Ex Situ ◽  
Temperature Dependent ◽  
Transmission Electron ◽  
Ion Energies

ABSTRACTIrradiation-induced amorphization of Cd2Nb2O7 pyrochlore was investigated by means of in-situ temperature-dependent ion-irradiation experiments in a transmission electron microscope, combined with ex-situ ion-implantation (at ambient temperature) and RBS/channeling analysis. The in-situ experiments were performed using Ne or Xe ions with energies of 280 and 1200 keV, respectively. For the bulk implantation experiments, the incident ion energies were 70 keV (Ne+) and 320 keV (Xe2+). The critical amorphization temperature for Cd2Nb2O7 is ∼480 K (280 keV Ne+) or ∼620 K (1200 keV Xe2+). The dose for in-situ amorphization at room temperature is 0.22 dpa for Xe2+, but is 0.65 dpa for Ne+ irradiation. Both types of experiments suggest a cascade overlap mechanism of amorphization. The results were analyzed in light of available models for the crystalline-to-amorphous transformation and were compared to previous ionirradiation experiments on other pyrochlore compositions.

scholarly journals Computer-Controlled Polishing System For Preparing Multiple Pre-FIB TEM Specimens

2007 ◽  
Vol 15 (6) ◽  
pp. 38-39
Author(s):  
D. J. MacMahon ◽  
E. Raz-Moyal
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Product Yield ◽  
Interface Layer ◽  
Ex Situ ◽  
Advantages And Disadvantages ◽  
Transmission Electron ◽  
Invaluable Tool ◽  
Electron Microscopes

Semiconductor manufacturers are increasingly turning to Transmission Electron Microscopes (TEMs) to monitor product yield and process control, analyze defects, and investigate interface layer morphology. To prepare TEM specimens, Focused Ion Beam (FIB) technology is an invaluable tool, yielding a standard milled TEM lamella approximately 15 μm wide, 5 μm deep and ~100 nm thick. Several techniques have been developed to extract these tiny objects from a large wafer and view it in the TEM. These techniques, including ex-situ lift-out, H-bar, and in-situ lift-out, have different advantages and disadvantages, but all require painstaking preparation of one specimen at a time.

scholarly journals Origin of the Difference in the Resistivity of As-Grown Focused-Ion- and Focused-Electron-Beam-Induced Pt Nanodeposits

2009 ◽  
Vol 2009 ◽  
pp. 1-11 ◽  
Author(s):  
J. M. De Teresa ◽  
R. Córdoba ◽  
A. Fernández-Pacheco ◽  
O. Montero ◽  
P. Strichovanec ◽  
...  
Keyword(s):  
Voltage Dependence ◽  
Ion Beam ◽  
Carbon Matrix ◽  
Ex Situ ◽  
Semiconducting Materials ◽  
Dual Beam ◽  
Transmission Electron ◽  
The Difference ◽  
Main Component

We study the origin of the strong difference in the resistivity of focused-electron- and focused-Ga-ion-beam-induced deposition (FEBID and FIBID, resp.) of Pt performed in a dual beam equipment using(CH3)3Pt(CpCH3)as the precursor gas. We have performed in-situ and ex-situ resistance measurements in both types of nanodeposits, finding that the resistivity of Pt by FEBID is typically four orders of magnitude higher than Pt by FIBID. In the case of Pt by FEBID, the current-versus-voltage dependence is nonlinear and the resistance-versus-temperature behavior is strongly semiconducting, whereas Pt by FIBID shows linear current-versus-voltage dependence and only slight temperature dependence. The microstructure, as investigated by high-resolution transmission electron microscopy, consists in all cases of Pt single crystals with size about 3 nm embedded in an amorphous carbonaceous matrix. Due to the semiconducting character of the carbon matrix, which is the main component of the deposit, we propose that the transport results can be mapped onto those obtained in semiconducting materials with different degrees of doping. The different transport properties of Pt by FEBID and FIBID are attributed to the higher doping level in the case of FIBID, as given by composition measurements obtained with energy-dispersive X-ray microanalysis.

scholarly journals Effects of the Surface on Displacement Cascades Produced by Heavy-Ion Irradiation of Ni3Al and Cu3Au

1996 ◽  
Vol 439 ◽  
Author(s):  
S. Müller ◽  
M. L. Jenkins ◽  
C. Abromeit ◽  
H. Wollenberger
Keyword(s):  
Ion Irradiation ◽  
Incident Angle ◽  
Ion Beam ◽  
Heavy Ion ◽  
Small Population ◽  
Dislocation Loops ◽  
Near Surface ◽  
Ion Energy ◽  
Heavy Ion Irradiation ◽  
Transmission Electron

AbstractStereo transmission electron microscopy has been used to characterise the distribution in depth of disordered zones and associated dislocation loops in the ordered alloys Ni3Al and Cu3Au after heavy ion irradiation, most extensively for Ni3Al irradiated with 50 keV Ta+ ions at a temperature of 573 K. The Cu3Au specimen was irradiated with 50 keV Ni+ ions at an incident angle of 45° at a temperature of 373 K. In Ni3Al the defect yield, i.e. the probability for a disordered zone to contain a loop was found to be strongly dependent on the depth of the zone in the foil, varying from about 0.7 for near-surface zones to about 0.2 in the bulk. The sizes and shapes of disordered zones were only weakly dependent on depth, except for a small population of zones very near the surface which were strongly elongated parallel to the incident ion beam. In Cu3Au the surface had a smaller but still significant effect on the defect yield. The dependence of the tranverse disordered zone diameter d on ion energy E for Ta+ irradiation of NiA was found to follow a relationship d = k1, E1/α with k, = 2.4 ± 0.4 and α = 3.3 ± 0.4. A similar relationship with the same value of α is valid for a wide variety of incident ion/target combinations found in the literature.

scholarly journals Effect of He-appm/DPA ratio on the damage microstructure of tungsten

MRS Advances ◽  
2016 ◽  
Vol 1 (42) ◽  
pp. 2893-2899 ◽  
Author(s):  
R.W. Harrison ◽  
H. Amari ◽  
G. Greaves ◽  
J.A. Hinks ◽  
S.E. Donnelly
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Irradiation ◽  
Dislocation Loops ◽  
Vacancy Clusters ◽  
Transmission Electron ◽  
Damage Structure ◽  
Ordered Array ◽  
20 Nm

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.

In-Situ Observation Of Aln Formation During Nitridation Of Sapphire By Ultrahigh Vacuum Transmission Electron Microscopy

1997 ◽  
Vol 482 ◽  
Author(s):  
M. Yeadon ◽  
M. T. Marshall ◽  
F. Hamdani ◽  
S. Pekin ◽  
H. Morkoc ◽  
...  
Keyword(s):  
Ultrahigh Vacuum ◽  
Ex Situ ◽  
In Situ Observation ◽  
Island Growth ◽  
Kinetic Measurements ◽  
Transmission Electron ◽  
Before And After ◽  
Subsequent Exposure ◽  
Diffraction Patterns

AbstractUsing a novel ultrahigh vacuum transmission electron microscope (UHV TEM) with insitu molecular beam epitaxy capability we have studied the nitridation of (0001) sapphire upon exposure to ammonia. Atomically flat sapphire surfaces for the experiments were obtained by high temperature annealing. Subsequent exposure to ammonia flow at 950°C led to the successful synthesis of epitaxial AIN; the films were characterized in-situ using TEM. Complimentary ex-situ atomic force microscopy (AFM) was also performed in order to characterize the surface morphology before and after nitridation.The experiments indicate that AIN grows by a 3D island growth mechanism. Electron diffraction patterns suggest an abrupt AIN/sapphire interface with no evidence of the formation of Al–O–N compounds. The rate limiting step in the nitridation reaction appears to be the diffusion of nitrogen and oxygen species between the free surface of the growing AIN film and the reaction interface. It is inferred from kinetic measurements that diffusion of these species occurs along the boundaries between coalescing AIN islands.

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