Jeffrey M. Wheeler

Elevated temperature, nano-mechanical testing in situ in the scanning electron microscope.

A general nano-mechanical test platform capable of performing variable temperature and variable strain rate testing in situ in the scanning electron microscope is described. A variety of test geometries are possible in combination with focused ion beam machining or other fabrication techniques: indentation, micro-compression, cantilever bending, and scratch testing. The system is intrinsically displacement-controlled, which allows it to function directly as a micro-scale thermomechanical test frame. Stable, elevated temperature indentation∕micro-compression requires the indenter tip and the sample to be in thermal equilibrium to prevent thermal displacement drift due to thermal expansion. This is achieved through independent heating and temperature monitoring of both the indenter tip and sample. Furthermore, the apex temperature of the indenter tip is calibrated, which allows it to act as a referenced surface temperature probe during contact. A full description of the system is provided, and the effects of indenter geometry and of radiation on imaging conditions are discussed. The stabilization time and temperature distribution throughout the system as a function of temperature is characterized. The advantages of temperature monitoring and thermal calibration of the indenter tip are illustrated, which include the possibility of local thermal conductivity measurement. Finally, validation results using nanoindentation on fused silica and micro-compression of [100] silicon micro-pillars as a function of temperature up to 500 °C are presented, and procedures and considerations taken for these measurements are discussed. A brittle to ductile transition from fracture to splitting then plastic deformation is directly observed in the SEM for silicon as a function of temperature.

Invited Article: Indenter materials for high temperature nanoindentation

As nanoindentation at high temperatures becomes increasingly popular, a review of indenter materials for usage at high temperatures is instructive for identifying appropriate indenter-sample materials combinations to prevent indenter loss or failure due to chemical reactions or wear during indentation. This is an important consideration for nanoindentation as extremely small volumes of reacted indenter material will have a significant effect on measurements. The high temperature hardness, elastic modulus, thermal properties, and chemical reactivities of diamond, boron carbide, silicon carbide, tungsten carbide, cubic boron nitride, and sapphire are discussed. Diamond and boron carbide show the best elevated temperature hardness, while tungsten carbide demonstrates the lowest chemical reactivity with the widest array of elements.

Elevated temperature,in situindentation with calibrated contact temperatures

Stable, elevated temperature indentation requires the indenter tip and the sample to be in thermal equilibrium to prevent thermal displacement drift due to thermal expansion. However, temperature feedback on the sample and/or indenter temperatures comes from thermocouples which are not generally located at the contacting surfaces. Thus, a temperature gradient exists between the thermocouple and the contact surfaces. In this work, two procedures for calibrating the surface temperature of the indenter tip via thermocouple indentation and Raman spectroscopy are demonstrated at temperatures between 25°C and 150°C. Good agreement is found between the two methods, and thermal drift is observed to be minimal at the calibrated temperatures. A linear relationship is also demonstrated between measured temperature shifts during contact and heat flow calculated from thermal conductivity, contact area and thermal gradient.

Measuring the fracture resistance of hard coatings

A way of characterizing cracking in a hard coating is described. Microscale double cantilever beams have been made by focused ion beam milling and compressed in situ using a nanoindenter. The method can account for frictional effects and is demonstrated first on single crystals of SiC and GaAs of known toughness, before studying cracking in CrN-based hard coatings. It is found that ultra-fine grained CrAlN/Si3N4 coatings have a toughness approximately twice that of a conventional CrN coating. Although grain-size effects are still unclear, in situ observations directly show crack interactions with particles of Cr and voids in the film.

Template‐Free 3D Microprinting of Metals Using a Force‐Controlled Nanopipette for Layer‐by‐Layer Electrodeposition

A novel 3D printing method for voxel-by-voxel metal printing is presented. Hollow atomic force microscopy (AFM) cantilevers are used to locally supply metal ions in an electrochemical cell, enabling a localized electroplating reaction. By exploiting the deflection feedback of these probes, electrochemical 3D metal printing is, for the first time, demonstrated in a layer-by-layer fashion, enabling the fabrication of arbitrary-shaped geometries.

Elevated temperature, strain rate jump microcompression of nanocrystalline nickel

Nanocrystalline and ultrafine-grained materials show enhanced strain rate sensitivity (SRS) in comparison to their coarse grained counterparts. Majority of SRS measurements on nanocrystalline thin films reported in literature have focused on nanoindentation-based approaches. In this paper, micropillar strain rate jump tests were demonstrated on an electrodeposited nanocrystalline nickel film from 25 to 100 °C. SRS exponent, m, and activation volume, V, values were determined as a function of temperature. The measured values were found to be in good agreement with previously reported literature on bulk and nanoindentation measurements. Apparent activation energy for deformation was found to be about 100 kJ/mol, which is close to that for grain boundary diffusion in nickel. Grain boundary sliding was observed in the deformed pillars from scanning electron microscopy images.

Nanocrystalline High-Entropy Alloys: A New Paradigm in High-Temperature Strength and Stability

Metals with nanometer-scale grains or nanocrystalline metals exhibit high strengths at ambient conditions, yet their strengths substantially decrease with increasing temperature, rendering them unsuitable for usage at high temperatures. Here, we show that a nanocrystalline high-entropy alloy (HEA) retains an extraordinarily high yield strength over 5 GPa up to 600 °C, 1 order of magnitude higher than that of its coarse-grained form and 5 times higher than that of its single-crystalline equivalent. As a result, such nanostructured HEAs reveal strengthening figures of merit-normalized strength by the shear modulus above 1/50 and strength-to-density ratios above 0.4 MJ/kg, which are substantially higher than any previously reported values for nanocrystalline metals in the same homologous temperature range, as well as low strain-rate sensitivity of ∼0.005. Nanocrystalline HEAs with these properties represent a new class of nanomaterials for high-stress and high-temperature applications in aerospace, civilian infrastructure, and energy sectors.

Small-scale fracture toughness of ceramic thin films: the effects of specimen geometry, ion beam notching and high temperature on chromium nitride toughness evaluation

Abstract For the implementation of thin ceramic hard coatings into intensive application environments, the fracture toughness is a particularly important material design parameter. Characterisation of the fracture toughness of small-scale specimens has been a topic of great debate, due to size effects, plasticity, residual stress effects and the influence of ion penetration from the sample fabrication process. In this work, several different small-scale fracture toughness geometries (single-beam cantilever, double-beam cantilever and micro-pillar splitting) were compared, fabricated from a thin physical vapour-deposited ceramic film using a focused ion beam source, and then the effect of the gallium-milled notch on mode I toughness quantification investigated. It was found that notching using a focused gallium source influences small-scale toughness measurements and can lead to an overestimation of the fracture toughness values for chromium nitride (CrN) thin films. The effects of gallium ion irradiation were further studied by performing the first small-scale high-temperature toughness measurements within the scanning electron microscope, with the consequence that annealing at high temperatures allows for diffusion of the gallium to grain boundaries promoting embrittlement in small-scale CrN samples. This work highlights the sensitivity of some materials to gallium ion penetration effects, and the profound effect that it can have on fracture toughness evaluation.

Approaching the Limits of Strength: Measuring the Uniaxial Compressive Strength of Diamond at Small Scales

Diamond ⟨100⟩- and ⟨111⟩-oriented nanopillars were fabricated by focused ion beam (FIB) milling from synthetic single crystals and compressed using a larger diameter diamond punch. Uniaxial compressive failure was observed via fracture with a plateau in maximum stress of ∼0.25 TPa, the highest uniaxial strength yet measured. This corresponded to maximum shear stresses that converged toward 75 GPa or ∼ G/7 at small sizes, which are very close to the ultimate theoretical yield stress estimate of G/2π.

The effect of size on the strength of FCC metals at elevated temperatures: annealed copper

Abstract As the length scale of sample dimensions is reduced to the micron and sub-micron scales, the strength of various materials has been observed to increase with decreasing size, a fact commonly referred to as the ‘sample size effect’. In this work, the influence of temperature on the sample size effect in copper is investigated using in situ microcompression testing at 25, 200 and 400 °C in the SEM on vacuum-annealed copper structures, and the resulting deformed structures were analysed using X-ray μLaue diffraction and scanning electron microscopy. For pillars with sizes between 0.4 and 4 μm, the size effect was measured to be constant with temperature, within the measurement precision, up to half of the melting point of copper. It is expected that the size effect will remain constant with temperature until diffusion-controlled dislocation motion becomes significant at higher temperatures and/or lower strain rates. Furthermore, the annealing treatment of the copper micropillars produced structures which yielded at stresses three times greater than their un-annealed, FIB-machined counterparts.