Graphene application within electrochemical sensing has been widely reported, but mainly as a composite, which adds summative effects to an underlying electrode. In this work we report the use of laser-scribed graphene as a distinct electrode patterned on a non-conducting flexible substrate. The laser-scribed graphene electrode compared favourably to established carbon macroelectrodes when evaluating both inner sphere and outer sphere redox probes, providing promise of extensive utility as an electrochemical sensor. The laser-scribed graphene electrode demonstrated the fastest heterogeneous electron transfer rate of all the electrodes evaluated with a k(0) of 0.02373 cm s(-1) for potassium ferricyanide, which exceeds commercially available edge plane pyrolytic graphite at 0.00260 cm s(-1), basal plane pyrolytic graphite at 0.00033 cm s(-1) and the very slow and effectively irreversible electrochemistry observed using single layer graphene. Finally and most significantly, a proof of principle system was fabricated using the laser-scribed graphene as working electrode, counter electrode and underlying base for the Ag/AgCl reference electrode, all in situ on the same planar flexible substrate, removing the requirement of macroscale external electrodes. The planar three electrode format operated with the same optimal electrode characteristics. Furthermore, the fabrication is inexpensive, scalable and compatible with a disposable biosensor format, considerably widening the potential applications in electrochemical bio-sensing for laser-scribed graphene.
Calibration of atomic force microscope (AFM) cantilevers is necessary for the measurement of nanonewton and piconewton forces, which are critical to analytical applications of AFM in the analysis of polymer surfaces, biological structures and organic molecules at nanoscale lateral resolution. We have developed a compact and easy-to-use reference artefact for this calibration, using a method that allows traceability to the SI (Système International). Traceability is crucial to ensure that force measurements by AFM are comparable to those made by optical tweezers and other methods. The new non-contact calibration method measures the spring constant of these artefacts, by a combination of electrical measurements and Doppler velocimetry. The device was fabricated by silicon surface micromachining. The device allows AFM cantilevers to be calibrated quite easily by the 'cantilever-on-reference' method, with our reference device having a spring constant uncertainty of around ± 5% at one standard deviation. A simple substitution of the analogue velocimeter used in this work with a digital model should reduce this uncertainty to around ± 2%. Both are significant improvements on current practice, and allow traceability to the SI for the first time at these nanonewton levels.
Calibration of atomic force microscope (AFM) cantilevers is necessary for the measurement of nanonewton and piconewton forces, which are critical to analytical applications of AFM in the analysis of polymer surfaces, biological structures and organic molecules. We have developed a compact and easy-to-use reference artefact for this calibration by bulk micromachining of silicon, which we call a cantilever microfabricated array of reference springs (C-MARS). Two separate reference cantilever structures, each nominally 3 µm thick, are fabricated from a single crystal silicon membrane. A binary code of surface oxide squares (easily visible in light, electron and atomic force microscopy) makes it easy to locate the position of the AFM tip along the length of the cantilevers. Uncertainty in location is the main source of error when calibrating an AFM using reference cantilevers, especially for those having spring constants greater than around 10 N m −1. This error is effectively eliminated in our new design. The C-MARS device spans the range of spring constants from 25 N m −1 down to 0.03 N m −1 important in AFM, allowing almost any contact-mode AFM cantilever to be calibrated easily and rapidly.
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