J. A. Hinks

In-situ TEM observation of the response of ultrafine- and nanocrystalline-grained tungsten to extreme irradiation environments

The accumulation of defects, and in particular He bubbles, can have significant implications for the performance of materials exposed to the plasma in magnetic-confinement nuclear fusion reactors. Some of the most promising candidates for deployment into such environments are nanocrystalline materials as the engineering of grain boundary density offers the possibility of tailoring their radiation resistance properties. In order to investigate the microstructural evolution of ultrafine- and nanocrystalline-grained tungsten under conditions similar to those in a reactor, a transmission electron microscopy study with in situ 2 keV He+ ion irradiation at 950°C has been completed. A dynamic and complex evolution in the microstructure was observed including the formation of defect clusters, dislocations and bubbles. Nanocrystalline grains with dimensions less than around 60 nm demonstrated lower bubble density and greater bubble size than larger nanocrystalline (60–100 nm) and ultrafine (100–500 nm) grains. In grains over 100 nm, uniform distributions of bubbles and defects were formed. At higher fluences, large faceted bubbles were observed on the grain boundaries, especially on those of nanocrystalline grains, indicating the important role grain boundaries can play in trapping He and thus in giving rise to the enhanced radiation tolerance of nanocrystalline materials.

MIAMI: Microscope and ion accelerator for materials investigations

A transmission electron microscope (TEM) with in situ ion irradiation has been built at the University of Salford, U.K. The system consists of a Colutron G-2 ion source connected to a JEOL JEM-2000FX TEM via an in-house designed and constructed ion beam transport system. The ion source can deliver ion energies from 0.5 to 10 keV for singly charged ions and can be floated up to 100 kV to allow acceleration to higher energies. Ion species from H to Xe can be produced for the full range of energies allowing the investigation of implantation with light ions such as helium as well as the effects of displacing irradiation with heavy inert or self-ions. The ability to implant light ions at energies low enough such that they come to rest within the thickness of a TEM sample and to also irradiate with heavier species at energies sufficient to cause large numbers of atomic displacements makes this facility ideally suited to the study of materials for use in nuclear environments. TEM allows the internal microstructu...

Reversible Loss of Bernal Stacking during the Deformation of Few-Layer Graphene in Nanocomposites

The deformation of nanocomposites containing graphene flakes with different numbers of layers has been investigated with the use of Raman spectroscopy. It has been found that there is a shift of the 2D band to lower wavenumber and that the rate of band shift per unit strain tends to decrease as the number of graphene layers increases. It has been demonstrated that band broadening takes place during tensile deformation for mono- and bilayer graphene but that band narrowing occurs when the number of graphene layers is more than two. It is also found that the characteristic asymmetric shape of the 2D Raman band for the graphene with three or more layers changes to a symmetrical shape above about 0.4% strain and that it reverts to an asymmetric shape on unloading. This change in Raman band shape and width has been interpreted as being due to a reversible loss of Bernal stacking in the few-layer graphene during deformation. It has been shown that the elastic strain energy released from the unloading of the inner graphene layers in the few-layer material (∼0.2 meV/atom) is similar to the accepted value of the stacking fault energies of graphite and few layer graphene. It is further shown that this loss of Bernal stacking can be accommodated by the formation of arrays of partial dislocations and stacking faults on the basal plane. The effect of the reversible loss of Bernal stacking upon the electronic structure of few-layer graphene and the possibility of using it to modify the electronic structure of few-layer graphene are discussed.

In-situ observation and atomic resolution imaging of the ion irradiation induced amorphisation of graphene

Ion irradiation has been observed to induce a macroscopic flattening and in-plane shrinkage of graphene sheets without a complete loss of crystallinity. Electron diffraction studies performed during simultaneous in-situ ion irradiation have allowed identification of the fluence at which the graphene sheet loses long-range order. This approach has facilitated complementary ex-situ investigations, allowing the first atomic resolution scanning transmission electron microscopy images of ion-irradiation induced graphene defect structures together with quantitative analysis of defect densities using Raman spectroscopy.

Grain Size Threshold for Enhanced Irradiation Resistance in Nanocrystalline and Ultrafine Tungsten

ABSTRACT Nanocrystalline metals are considered highly radiation-resistant materials due to their large grain boundary areas. Here, the existence of a grain size threshold for enhanced irradiation resistance in high-temperature helium-irradiated nanocrystalline and ultrafine tungsten is demonstrated. Average bubble density, projected bubble area and the corresponding change in volume were measured via transmission electron microscopy and plotted as a function of grain size for two ion fluences. Nanocrystalline grains of less than 35 nm size possess ∼10–20 times lower change in volume than ultrafine grains and this is discussed in terms of the grain boundaries defect sink efficiency. GRAPHICAL ABSTRACT IMPACT STATEMENT A grain size threshold in nanocrystalline and ultrafine tungsten has been shown to exist for enhanced irradiation-resistance performance during high-temperature helium irradiation.

Helium irradiation effects in polycrystalline Si, silica, and single crystal Si

Transmission electron microscopy (TEM) has been used to investigate the effects of room temperature 6 keV helium ion irradiation of a thin (≈55 nm thick) tri-layer consisting of polycrystalline Si, silica, and single-crystal Si. The ion irradiation was carried out in situ within the TEM under conditions where approximately 24% of the incident ions came to rest in the specimen. This paper reports on the comparative development of irradiation-induced defects (primarily helium bubbles) in the polycrystalline Si and single-crystal Si under ion irradiation and provides direct measurement of a radiation-induced increase in the width of the polycrystalline layer and shrinkage of the silica layer. Analysis using TEM and electron energy-loss spectroscopy has led to the hypothesis that these result from helium-bubble-induced swelling of the silicon and radiation-induced viscoelastic flow processes in the silica under the influence of stresses applied by the swollen Si layers. The silicon and silica layers are sputt...

Transmission Electron Microscopy Study of Graphite under in situ Ion Irradiation

Graphite is employed as a moderator and structural component in 18 of the United Kingdoms fleet of Magnox and Advanced Gas-cooled Reactors (AGRs). During the operational lifetime of a reactor, graphite undergoes complex physical and mechanical property changes including dimensional modification, owing to the effects of temperature, oxidation and irradiation-induced atomic displacements. In order to safely extend the lifetime of the current fleet of AGRs, and also to develop materials for GenIV concepts such as the Very-High- Temperature Reactor (VHTR), it is important to gain a better understanding of the fundamental atomic processes which underpin the behaviour of graphite under current and future operational conditions. This study has focused on the effects of temperature and displacing radiation on the evolution of Mrozowski cracks in highly-orientated pyrolytic graphite (HOPG) using the new Microscope and Ion Accelerator for Materials Investigations (MIAMI) facility. This instrument allows transmission electron microscopy to be performed in situ whilst simultaneously ion irradiating to radiation damage levels typically reached in a reactor. By using this technique, it is possible to explore the development of radiation damage under a range of different conditions continuously from start-to-finish rather than just observing the end-states accessible in ex situ studies.

Engineering self-organising helium bubble lattices in tungsten

The self-organisation of void and gas bubbles in solids into superlattices is an intriguing nanoscale phenomenon. Despite the discovery of these lattices 45 years ago, the atomistics behind the ordering mechanisms responsible for the formation of these nanostructures are yet to be fully elucidated. Here we report on the direct observation via transmission electron microscopy of the formation of bubble lattices under He ion bombardment. By careful control of the irradiation conditions, it has been possible to engineer the bubble size and spacing of the superlattice leading to important conclusions about the significance of vacancy supply in determining the physical characteristics of the system. Furthermore, no bubble lattice alignment was observed in the <111> directions pointing to a key driving mechanism for the formation of these ordered nanostructures being the two-dimensional diffusion of self-interstitial atoms.

An in-situ TEM investigation of He bubble evolution in SiC

This paper presents work using the capabilities of two TEM with in-situ ion irradiation facilities: Microscope and Ion Accelerator for Materials Investigation (MIAMI) at the University of Huddersfield and Joint Accelerators for Nano-science and Nuclear Simulation JANNuS at Centre de Spectrometrie Nucleaire et de Spectrometrie de Masse (CSNSM), Orsay, France, to study the nucleation and growth of He bubbles in silicon carbide (SiC) and to carry out an investigation into bubble behaviour at high temperatures and under displacing irradiation. Preliminary results on bubble nucleation and growth during He irradiation of SiC are presented together with results from a simultaneous anneal and high-energy heavy-ion irradiation of samples containing He bubbles. The displacing irradiation is observed to impede He bubble growth resulting in smaller bubbles than those obtained from an anneal alone. A tentative interpretation of these observations is presented.

Transmission electron microscopy of the amorphization of copper indium diselenide by in situ ion irradiation

Copper indium diselenide (CIS), along with its derivatives Cu(In,Ga)(Se,S)2, is a prime candidate for use in the absorber layers of photovoltaic devices. Due to its ability to resist radiation damage, it is particularly well suited for use in extraterrestrial and other irradiating environments. However, the nature of its radiation hardness is not well understood. In this study, transmission electron microscopy (TEM) with in situ ion irradiation was used to monitor the dynamic microstructural effects of radiation damage on CIS. Samples were bombarded with 400 keV xenon ions to create large numbers of atomic displacements within the thickness of the TEM samples and thus explore the conditions under which, if any, CIS could be amorphized. By observing the impact of heavily damaging radiation in situ—rather than merely the end-state possible in ex situ experiments—at the magnifications allowed by TEM, it was possible to gain an understanding of the atomistic processes at work and the underlying mechanism that...