Four different conductive supports are analysed regarding their suitability for combined atomic force and scanning electrochemical microscopy (AFM-SECM) on biological membranes. Highly oriented pyrolytic graphite (HOPG), MoS(2), template stripped gold, and template stripped platinum are compared as supports for high resolution imaging of reconstituted membrane proteins or native membranes, and as electrodes for transferring electrons from or to a redox molecule. We demonstrate that high resolution topographs of the bacterial outer membrane protein F can be recorded by contact mode AFM on all four supports. Electrochemical feedback experiments with conductive cantilevers that feature nanometre-scale electrodes showed fast re-oxidation of the redox couple Ru(NH(3))(6)(3+/2+) with the two metal supports after prolonged immersion in electrolyte. In contrast, the re-oxidation rates decayed quickly to unpractical levels with HOPG or MoS(2) under physiological conditions. On HOPG we observed heterogeneity in the re-oxidation rate of the redox molecules with higher feedback currents at step edges. The latter results demonstrate the capability of conductive cantilevers with small electrodes to measure minor variations in an SECM signal and to relate them to nanometre-scale features in a simultaneously recorded AFM topography. Rapid decay of re-oxidation rate and surface heterogeneity make HOPG or MoS(2) less attractive for combined AFM-SECM experiments on biological membranes than template stripped gold or platinum supports.

A combined atomic force and scanning electrochemical microscope probe is presented. The probe is electrically insulated except at the very apex of the tip, which has a radius of curvature in the range of 10-15 nm. Steady-state cyclic voltammetry measurements for the reduction of Ru(NH3)6Cl3 and feedback experiments showed a distinct and reproducible response of the electrode. These experimental results agreed with finite element simulations for the corresponding diffusion process. Sequentially topographical and electrochemical studies of Pt lines deposited onto Si3N4 and spaced 100 nm apart (edge to edge) showed a lateral electrochemical resolution of 10 nm.

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Well-controlled spherical microstructures open new possibilities for several MEMS devices, such as hemispherical microfluidic channels or micro-optical elements. However, machining of micro-spherical shapes has proven to be difficult with conventional planar micro-fabrication processes. This paper presents a fabrication method allowing the fabrication of controlled micro-spherical cap structures with defined edge angles. Drops of 30 pL of an epoxy solution were accurately inkjet printed on circular platforms. The deposited volume is confined by the rim of the platforms. This allows a fine tuning of the spherical cap edge angle as well as its height and radius of curvature. The presented method allowed fabricating large arrays of well-controlled micro-spherical shapes of different diameters, ranging from 50 to 930 μm, with a maximum controlled edge angle tuning of 85 • . Theoretical investigations of the underlying phenomena are also presented. Good agreement between experimental results and theoretical expectations has been observed, with standard deviations below 3%. Using the proposed method, several 2D arrays up to 900 micro hemispheres with an edge angle of 90 • ± 2 • have been fabricated with a yield above 98%.

This paper describes the characterization and application of electrically insulated conductive tips mounted on a cantilever for use in an atomic force microscope and operated in liquid. These multifunctional probes were microfabricated and designed for measurements on biological samples in buffer solution, but they can also be employed for electrochemical applications, in particular scanning electrochemical microscopy. The silicon nitride based cantilevers had a spring constant ≤0.1 N m−1 and a conductive tip, which was insulated except at the apex. The conductive core of the tip consisted of a metal, e.g. platinum silicide, and exhibited a typical radius of 15 nm. The mechanical and electrical characterization of the probe is presented and discussed. First measurements on the hexagonally packed intermediate layer of Deinococcus radiodurans demonstrated the possibility to adjust the image contrast by applying a voltage between a support and the conductive tip and to measure variations of less than 1 pA in faradaic current with a lateral resolution of 7.8 nm.