David E.J. Armstrong

Micro-mechanical measurements of fracture toughness of bismuth embrittled copper grain boundaries

Measuring the fracture properties of single grain boundaries has until now required macroscopic bi-crystals which are expensive and not always available. We describe a method for fracture testing using micro-cantilevers, manufactured using focussed ion beam machining and tested using a nanoindenter. We have used the method to measure the fracture toughness of selected grain boundaries in bismuth-embrittled copper. This technique is applicable to grain boundaries in other brittle polycrystalline samples for which large bi-crystals cannot be produced for conventional testing.

Effects of sequential tungsten and helium ion implantation on nano-indentation hardness of tungsten

To simulate neutron and helium damage in a fusion reactor first wall sequential self-ion implantation up to 13 dpa followed by helium-ion implantation up to 3000 appm was performed to produce damaged layers of ∼2 μm depth in pure tungsten. The hardness of these layers was measured using nanoindentation and was studied using transmission electron microscopy. Substantial hardness increases were seen in helium implanted regions, with smaller hardness increases in regions which had already been self-ion implanted, thus, containing pre-existing dislocation loops. This suggests that, for the same helium content, helium trapped in distributed vacancies gives stronger hardening than helium trapped in vacancies condensed into dislocation loops.

Nanoindentation and micromechanical testing of iron-chromium alloys implanted with iron ions

The mechanical properties of Fe-Cr alloys were investigated in as-grown and in post-ion-implanted conditions. Sets of specimens were produced using dual implantations of Fe+ ions to give 1µm deep damaged layers with average damage levels of 0.35 displacements per atom and 5.33 displacements per atom. Nanoindentation was used to measure hardness as a function of depth and showed that implanted material had a higher hardness than unimplanted material. Additionally, micron-scale cantilevers were fabricated from the ion-damaged surface of the material and were tested using a nanoindenter for AFM-imaging and loading. The mechanical properties deduced from the controlled loading of these cantilevers pertain only to radiation-damaged material, and for the high-dose material show significant changes in Young’s modulus, yield stress and work-hardening.

The micro-mechanical properties of ion irradiated tungsten

Micro-mechanical testing techniques have proved successful in extracting the properties of bulk materials from small-scale tests. In particular, focussed ion beam (FIB)-machined micro-cantilevers have been shown to produce quantitative, accurate modulus values when used on materials such as pure copper or silicon. In this work, this technique is extended to study the micro-mechanical properties of ion-irradiated, commercially pure tungsten. Ion irradiation has been used to model the cascade damage produced by fusion neutrons in tungsten. Due to the small depth of ion-implanted layers, micro-mechanical tests must be carried out to determine the mechanical properties of the material. These cantilever tests and additional nanoindentation produces data comparable with literature data. An increase in hardness after implantation is measured, while the yield stress of the material remains unchanged. Helium implantation has an effect on the mechanical properties of tungsten. It is hypothesized that this is due to a change in the damage formed under irradiation, from dislocation loops formed in self-ion irradiation to helium-filled vacancies in simultaneous irradiation.

Hybrid electrolytes with 3D bicontinuous ordered ceramic and polymer microchannels for all-solid-state batteries

Hybrid solid electrolytes, composed of 3D ordered bicontinuous conducting ceramic and insulating polymer microchannels are reported. The ceramic channels provide continuous, uninterrupted pathways, maintaining high ionic conductivity between the electrodes, while the polymer channels permit improvement of the mechanical properties from that of the ceramic alone, in particular mitigation of the ceramic brittleness. The conductivity of a ceramic electrolyte is usually limited by resistance at the grain boundaries, necessitating dense ceramics. The conductivity of the 3D ordered hybrid is reduced by only the volume fraction occupied by the ceramic, demonstrating that the ceramic channels can be sintered to high density similar to a dense ceramic disk. The hybrid electrolytes are demonstrated using the ceramic lithium ion conductor Li1.4Al0.4Ge1.6(PO4)3 (LAGP). Structured LAGP 3D scaffolds with empty channels were prepared by negative replication of a 3D printed polymer template. Filling the empty channels with non-conducting polypropylene (PP) or epoxy polymer (epoxy) creates the structured hybrid electrolytes with 3D bicontinuous ceramic and polymer microchannels. Printed templating permits precise control of the ceramic to polymer ratio and the microarchitecture; as demonstrated by the formation of cubic, gyroidal, diamond and spinodal (bijel) structures. The electrical and mechanical properties depend on the microarchitecture, the gyroid filled with epoxy giving the best combination of conductivity and mechanical properties. An ionic conductivity of 1.6 × 10−4 S cm−1 at room temperature was obtained, reduced from the conductivity of a sintered LAGP pellet only by the volume fraction occupied by the ceramic. The mechanical properties of the gyroid LAGP–epoxy electrolyte demonstrate up to 28% higher compressive failure strain and up to five times the flexural failure strain of a LAGP pellet before rupture. Notably, this demonstrates that ordered ceramic and polymer hybrid electrolytes can have superior mechanical properties without significantly compromising ionic conductivity, which addresses one of the key challenges for all-solid-state batteries.

Extreme nanomechanics: vacuum nanoindentation and nanotribology to 950 °C

Elevated temperature mechanical and tribological properties can be more relevant for practical wear situations than corresponding measurements at room temperature. However, high temperature nanomechanics and nanotribology is highly challenging experimentally. To overcome these challenges the NanoTest*** has been developed with active heating of the indenter and sample with resistive heaters, horizontal loading, patented thermal control method and stage design. By separately actively heating*** and controlling the temperatures of indenter and sample their temperatures can be precisely matched so that there is no heat flow and minimal/no thermal drift during the high temperature indentation,*** and measurements can be performed as reliably as at room temperature. Above 500 °C it is beneficial to use a cubic Boron Nitride indenter with gas purging to limit oxidation of samples. To achieve higher temperatures without indenter or sample oxidation an ultra-low drift high temperature vacuum nanomechanics/tribology system capable of testing to*** much higher temperatures has been recently developed (NanoTest Xtreme). The influence of time-dependent deformation on elevated temperature nanomechanical behaviour is discussed, using published results in Argon on glass-ceramic solid oxide fuel cell seal materials and previously unpublished nanoindentation measurements on single crystal silicon and polycrystalline tungsten using the NanoTest Xtreme in vacuum at temperatures up to 950 °C. Studies of the elevated temperature nano-/micro-tribological*** behaviour of wear-resistant*** nitride-based and MAX-phase coatings are also briefly reviewed.

Micro-Fracture Testing of Ni-W Microbeams Produced by Electrodeposition and FIB Machining

Electrodeposited nickel-tungsten alloys are being considered as a candidate material for components for microelectromechanical systems (MEMS) fabricated by the LIGA (German acronym for lithography, electrodeposition, and forming) technology. In spite of having a useful range of properties including; hardness and strength, better tribological and chemical resistance and improved high temperature resistance as compared with the conventionally used electrodeposited Ni, these alloys possess certain brittleness. In this study, the fracture toughness of Ni-17.5 at%W alloy microcantilever beams (dimension: 60μm x 20μm x 14μm) fabricated by UV lithography and electrodeposition and notched by focused ion beam machining is investigated. Load was applied to the beams using a nanoindenter, which also allowed accurate positioning of the sample. Fracture toughness was calculated from the fracture load assuming a linear elastic behaviour. The Ni-W alloy beams were found to possess a mean fracture toughness of 2.97 MPa √m. The fracture toughness of Ni-W alloy is found to be higher than that of Si – another important MEMS material, but considerably lower than that of electrodeposited nickel and nickel base alloys.

Size effects resolve debate in 40 years of work on low-temperature plasticity in olivine

When deforming by low-temperature plasticity, the strength of the mantle mineral olivine is controlled by its grain size. The strength of olivine at low temperatures and high stresses in Earth’s lithospheric mantle exerts a critical control on many geodynamic processes, including lithospheric flexure and the formation of plate boundaries. Unfortunately, laboratory-derived values of the strength of olivine at lithospheric conditions are highly variable and significantly disagree with those inferred from geophysical observations. We demonstrate via nanoindentation that the strength of olivine depends on the length scale of deformation, with experiments on smaller volumes of material exhibiting larger yield stresses. This “size effect” resolves discrepancies among previous measurements of olivine strength using other techniques. It also corroborates the most recent flow law for olivine, which proposes a much weaker lithospheric mantle than previously estimated, thus bringing experimental measurements into closer alignment with geophysical constraints. Further implications include an increased difficulty of activating plasticity in cold, fine-grained shear zones and an impact on the evolution of fault surface roughness due to the size-dependent deformation of nanometer- to micrometer-sized asperities.

An Investigation into Fracture of Multi-Crystalline Silicon

As the thickness of multi-crystalline silicon solar cells continues to reduce, understanding the mechanical properties of the material is of increasing importance. In this study, a variety of techniques are used to study multi-crystalline silicon. Fracture tests are performed using four- and three-point bending. The fracture stress of as-sawn material reduces with increasing beam width and is increased in beams with a polished front surface. This indicates that fracture initiates from surface flaws. Modifications to standard fracture testing, including testing under liquid, are made so that beams fracture into just two pieces. By determining the crystallography either side of the location of fracture, multi-crystalline silicon was found to fail by transgranular fracture in the samples studied. Further evidence for this is gained from indentation experiments at grain boundaries. In order to understand the relative strength of grain boundaries, new approaches need to be considered. Therefore, a novel micromechanical technique, which enables individual grain boundaries to be studied, has started to be applied to multi-crystalline silicon. A focused ion beam is used to mill micron-scale cantilevers across notched grain boundaries, which are then loaded to fracture using the tip of a nanoindenter. The technique is shown to reproduce the known fracture toughness of {110} planes in single-crystal silicon, giving a value of 0.7 ± 0.3MPam1/2. Preliminary results are presented for fracture of multi-crystalline silicon.