Measuring coefficient of thermal expansion of materials of micrometre size using SEM/FIB microscope with in situ MEMS heating stage

A new method is proposed to measure the linear coefficient of thermal expansion (CTE) of solid metals and ceramics of micron‐sized dimensions. This approach uses a focused ion beam (FIB) to extract and transfer a slab of the sample, typically (15–20) ×10 × (3–5) µm onto a Micro‐Electro‐Mechanical Systems (MEMS) in situ heating holder inside a scanning electron microscope (SEM). CTE is thereafter calculated by image correlating the change of length (ΔL) between the fiducial marks on the slab as a function of temperature, taking advantage of the temperature calibration of the MEMS heating holder and nanometre resolution of the scanning electron microscope. The CTE results are validated to be consistent with standard copper and silicon. We further demonstrate the method on a graphene platelet reinforced copper composite and a graphite filler phase isolated from a bulk sample, these represent materials that cannot be practically synthesised or isolated at the macro‐scale. Errors associated with the measurement are discussed.