High-resolution electron microscope studies of irradiation-induced crystalline-to-amorphous transition in boron carbide

Abstract

The crystalline-to-amorphous (C-A) transition in boron carbide induced by 2 MeV electron irradiation was studied by high-resolution electron microscopy. It is revealed that the C-A transition takes place not homogeneously but heterogeneously over the irradiated volume and the volume fraction of the amorphous phase continuously increases with increasing dose of electrons.     

Formation of stacking fault tetrahedra around α-Fe particles in a Cu–Fe alloy

Abstract

The formation of stacking fault tetrahedra in a Cu–Fe alloy containing α-Fe particles has been examined by in situ observation in a high-vacuum and high-voltage electron microscope. A sudden disappearance of secondary defect contrast has been noted during prolonged electron irradiation. Concurrently, a moiré pattern develops inside the α-Fe, indicating the alignment of the low-index direction along the electron beam by rotation of the particles.     

Solid-phase epitaxy of implanted silicon at liquid nitrogen and room temperature induced by electron irradiation in the electron microscope

Abstract

Electron-beam-induced solid-phase epitaxy (SPE) has been obtained on cross-sections of implanted Si layers, by in situ irradiation in the electron microscope, with electrons of energies of 200, 250 and 300 keV, at both room and liquid-nitrogen temperature. The, absence of a transition from SPE to layer-by-layer amorphization (which is observed during ion-beam irradiation on decreasing the temperature below a certain critical value) and the athemal nature of the electron-induced crystallization process below room temperature, indicate that, although elastic displacement is the basic mechanism of both processes, the models which describe ion-beam-induced epitaxy in the temperature range 200≤T≤400°C cannot be extrapolated to explain the results of electron irradiation below room temperature.     

A new modulated structure in GaN nanoparticles

A new modulated structure with a superlattice having parameters a = 2.209nm, b = 3.826nm, c = 1.037nm and f = g = n = 90 has been found in GaN nanoparticles synthesized by a dc arc plasma method. The nanoparticles transformed further into particles with holes at their centres under electron-beam irradiation during high-resolution electron microscopy observations. At the same time, Ga atoms were extruded on to the surface of the nanoparticles and formed an amorphous layer. A series of simulations of high-resolution images and electron diffraction patterns revealed that the modulation could be attributed to aggregations of N vacancies founded during the electron bombardment. Molecular mechanics calculations show that the aggregation of N vacancies is far more energetically favourable than that of Ga vacancies. The stability of the GaN particles is discussed.     

Depth distribution of oxygen vacancies in 1 MeV Li + -irradiated KTiOPO 4

Electron-energy-loss spectra have been recorded from cross-sectional transmission electron microscopy samples of Li + -irradiated KTiOPO 4 single crystals. By evaluating the intensity in the pre-edge shoulder of the OK ionization edge, the depth distribution of O vacancies in radiation-damaged KTiOPO 4 was monitored. Li + irradiation at 295K and Li + irradiation at 100K generate very similar defect profiles except for an additional superficial maximum in the room-temperature-irradiated sample. Vacancy distributions in the O sublattice can be monitored on the nanometre scale by the method introduced. The methodology is potentially applicable to a wide range of materials, when pertinent defect-sensitive features in electron-energy-loss spectra are evaluated, and its sensitivity is expected to become further improved with the availability of monochromated electron sources in transmission electron microscopes.     

Atomistic study of structural fluctuations during radiation-induced amorphization in the ordered intermetallic compound NiTi

We have carried out an atomistic study of electron-induced amorphization of an ordered intermetallic compound NiTi by means of in-situ high-resolution high-voltage electron microscopy observations and molecular dynamics simulations. Both theoretical and experimental results show that metastable nanometre-size atomic clusters form and disappear during irradiation, so that a spatiotemporal fluctuation under amorphization is induced. Mean-lifetime measurements of these clusters demonstrate that high-energy particle irradiation provides a useful tool to study dynamic fluctuations of the local atomic structure in the non-equilibrium open systems.     

High-resolution electron microscopy of a microporous carbon

The structure of a microporous carbon prepared by the carbonization of sucrose was examined using high-resolution electron microscopy. It was found to be disordered and isotropic and primarily made up of tightly curved individual carbon layers, enclosing pores typically about 1nm in size. Completely closed carbon particles were also present. These observations suggest that the carbon may have a fullerene-related structure, in which pentagons and heptagons are distributed randomly throughout a hexagonal network, producing continuous curvature.     

Real temperature of nanoparticles in electron microscope beams

Abstract

This Letter presents a solution of the problem of the real temperature of nanoparticles under conditions of electron microscope beam irradiation. It is shown that the average temperature of the nanoparticles (NPs) may increase to several hundred degrees depending on contact conditions with the substrate, the intensity of the beam and the size of the NPs. The temperature increases with NP size a according to the dependence: T α a² for sufficiently small particles.     

Structure images of unaged martensite containing a high carbon content

Abstract

A highly tetragonal (large c/a ratio) martensite in a Fe-4 wt% Al-1·6 wt% Mn-2 wt% Calloy, which is not aged and considered to be as ‘fresh’ as possible, has been observed by high-resolution electron microscope. From the arrangement of atom rows in the [010] structure image and the corresponding electron diffraction pattern, it is concluded that carbon atoms are clustered on the (305) plane. The unit structure of these carbon-clustered regions is similar to that of the modulated structure observed in Fe-C alloys, although a periodic layer distribution of carbon atoms is not observed.     

Atomic and electronic structure of a carbon nitride compound prepared by magnetron sputtering

The atomic structure, chemical composition and chemical bonding state of a carbon nitride compound, synthesized by rf magnetron sputtering, have been studied by high-resolution electron microscopy, nanobeam diffraction and electron energy loss spectroscopy. It is revealed that the grain sizes of a crystalline compound in an amorphous matrix lie in the range 5-10 nm, and that the compound has a hexagonal structure with a = 0.324 nm and c = 0.404 nm. The C and N K edges are observed in the high-energy region of the electron-energy-loss spectrum. Only features corresponding to C sigma* bonds are found in the C K edge spectrum, which provides evidence for sp³ hybridization of C orbitals in the compound. Quantifying the electron-energy-loss spectra suggests that the compound is C₇N₁₀.     

Interrelated emission and spin–spin relaxation feature mediated by VO+ defects in Gd2O3 nanorods subjected to swift ion impact

We report on the manifestation and interconnected photoluminescence and electron paramagnetic resonance responses in gadolinium oxide (Gd₂O₃) nanorods subjected to 80 MeV carbon ion irradiation. On increasing the irradiation fluence between 1 × 10¹¹ and 3 × 10¹² ions/cm², the emission associated with neutral oxygen vacancies (V_Ox), positioned at ~350 nm, undergoes a steady increase compared to that associated with singly charged vacancies (V_O⁺), located at ~414 nm. The enhancement of spin–spin relaxation time (τ_ss) is ascribed to a substantial changeover from V_O⁺ to V_Ox defects with irradiation, the former being recognized as the major contributor to paramagnetic centres. Interconnected luminescence and spin–spin relaxation could provide insight for making advanced nanophosphors and spin valve elements.     

ω phase in individual latent tracks induced by irradiation of α-titanium with megaelectronvolt fullerenes

Evidence is obtained for the existence of a hexagonal y phase in individual latent tracks (i.e. in the vicinity of the ion paths) induced in hcp f -Ti after irradiation at 80K at low fluences with 30MeV C 60 ions. The orientation relationships between the f and y phases are those previously observed by Dammak et al . in 1993 when the y phase is obtained after irradiation at high fluences with gigaelectronvolt monomers at low temperatures (i.e. (002) f ||(210) y and [100] f ||[001] y ). Parallel moiré fringes, due to the overlapping of the structure of the y phase with the f matrix, are observed in bright-field images obtained with (020) f (||(030) y ) reflection conditions. The spacing of these fringes is very close to the value of 3.2nm expected from the interplanar distances d f (020) and d y (030) . After irradiation at 300K, such fringes are also observed but the track structure cannot be established unambiguously. This dependence of the irradiation temperature is related to the temperature-pressure structural properties. The present transmission electron microscopy observations are compared with those obtained by Dammak et al . in 1996 and 1999 in the case of irradiation with gigaelectronvolt monomers for which it has been established that an overlapping of tracks is necessary to induce the f M y transformation.     

Effects of temperature and electron energy on the electron-irradiation-induced decomposition of sapphire

The effects of temperature and electron energy on the electron-irradiation-induced decomposition of sapphire have been investigated by in situ transmission electron microscopy (TEM). It was found that the decomposition rate of α-Al₂O₃ increased with increasing irradiation temperature and decreased with increasing acceleration voltage. The core-hole Auger decay process (K–F model), rather than knock-on displacement, is responsible for the decomposition of α-Al₂O₃ under electron irradiation.     

A first HREM observation of the ordered carbon sublattice in a transition-metal carbide (VC1-x)

Abstract

The microstructure of long-range-ordered vanadium carbides based on V₆C₅ has been analysed by means of high-resolution electron microscopy (HREM). Lattice images have been produced by including in the objective-aperture superlattice spots associated with the ordered distribution of vacancies in the interstitial carbon sublattice of these substoichiometric compounds: ‘perfectly’ ordered structures have been imaged, and a direct discussion of the experimental micrographs is made in terms of positions of the vacancy-containing columns. This HREM study will soon be extended to theinvestigation of various kinds of planar defects within differently annealed specimens.     

Quasi-two-dimensional or hcp palladium nanoparticles with host-guest interaction prepared at room temperature

Quasi-two-dimensional palladium nanoparticles with an average lateral dimension of 7 nm have been prepared by reduction of a PdCl₂ graphite intercalation compound precursor by lithium-diphenylide in tetrahydrofuran at room temperature. Selected-area electron diffraction patterns provide evidence that the palladium nanoparticles are hcp single-crystal particles. Owing to the template effect of the graphite lattice, the lattice parameter of palladium was found to have a strong relation with the graphite, and a 3a _graphite superstructure was inferred. The palladium structure is rotated by 30^o with regard to the carbon host lattice. Raman spectroscopy on this sample showed that a charge transfer between carbon and palladium occurs. The sample can be considered as a common Pd-graphite intercalation compound with palladium nanoparticles as guest. This behaviour is different from palladium nanoparticles prepared by hydrogen reduction at higher temperatures from the same precursor material. These particles may represent an early stage of nanoparticle formation.     

Secondary defects induced by ion and electron irradiation of GaSb

Secondary defects induced by ion and electron irradiation up to 6?dpa (displacements per atom) at liquid-nitrogen temperature in GaSb thin films are compared. For Sn ion (60?keV) irradiation, voids were observed. However, for high-energy electron (2?MeV) irradiation, interstitial-type dislocation loops were produced. The densities of voids and interstitial-type dislocation loops were almost equivalent (8?×?10¹⁴?voids/m² and 3?×?10¹⁴?loops/m²) after irradiations at the same damage level of 6?dpa. It is concluded that the formation of voids by ion irradiation follows the creation of localised vacancy defects in cascade damage.     

Adoption of near-coincident-site lattice orientations by contacting monolayer rafts of metallic nanoparticles with different superlattice periodicities

A hexagonal raft of monodisperse alkane-thiol-stabilized Au nanoparticles has been self-assembled from solution on to an amorphous C substrate and then subsequently a second layer of monodisperse but differently sized gold nanoparticles deposited on top of the first. Detailed analysis of electron micrographs obtained from various regions of this bilayer revealed the presence of several distinct epitaxial interface structures. A simple near-coincident-site lattice model is used to rationalize the existence of the observed characteristic nanoparticle interface structures.     

Modification of the optical band gap of polyethylene by irradiation with electrons and gamma rays

Irradiation of polymers has become an important technique in producing special materials for electronic applications. In this study, the effects of electron and gamma irradiation on ultra-high-molecular-weight polyethylene (UHMWPE) samples have been studied using UV–Vis absorption spectroscopy. The UHMWPE samples were irradiated with electron and gamma rays with doses ranging from 25 kGy up to 500 kGy. An increase in the optical absorption and a shifting from the UV–Vis towards longer wavelengths were observed. Concomitantly, a pronounced decrease in the optical band gap was recorded as a function of dose level. The optical band gap E _g varied from 2.86 eV for a pristine sample down to ～1.98 eV and ～2 eV for samples irradiated with gamma rays and electrons at the highest doses, respectively. A correlation between E _g and the number of carbon atoms N in a formed cluster is discussed in terms of a modified Tauc equation.     

On the determination of the nature of misfit dislocations in semiconductor strained-layer heterostructures

Abstract

The study of the mechanisms of formation of misfit dislocations in latticemismatched semiconductor interfaces requires a comprehensive characterization of these dislocations. In particular the determination of the sense of their Burgers vectors by transmission electron microscopy makes it possible to show that they contribute to removing part of the mismatched-induced interfacial strain. Furthermore the nature (αorβ) of the dislocations can then be determined. The different methods of determination of the sense of Burgers vectors are reviewed and then applied to InGaAs/GaAs superlattices.     

Origin of the initial rapid age hardening in an Al-1.7 at.% Mg-1.1 at.% Cu alloy

The origin of the rapid hardening which occurs during the initial ageing stage of an Al-1.7 at.% Mg-1.1 at.% Cu alloy has been investigated by the threedimensional atom-probe (3DAP) and transmission electron microscopy techniques. Although the rapid hardening reaction occurs within 1 min at 150 degrees C, no evidence for solute clusters or Guinier-Preston-Bagaryatsky (GPB) zones was detected using the 3DAP after this ageing time. When a short-term aged specimen is deformed and then aged at 150 degrees C, further rapid hardening occurs. This suggests that the rapid hardening is associated with a solutedislocation interaction. Uniform dispersions of Cu-Mg co-clusters do not occur until closer to the end of the hardness plateau and it is thought that these evolve into GPB zones during the second stage of the age-hardening process.