We have successfully sculptured a variety of copper films with open interconnected macroporous walls and nanoparticles using hydrogen bubbles as the dynamic template. In this process, the hydrogen bubbles arising from the electrochemical reduction of H + in the deposition process functioned as the dynamic template for metal electrodeposition. Cu was electrodeposited and grew within the interstitial spaces between the hydrogen bubbles to form a macroporous film of Cu nanoparticles on the substrate, showing a typical integration of micro-nanostructure. The pore diameters and wall thickness of the porous copper films were successfully tailored by adjusting the concentration of the electrodeposition electrolyte, the applied current density, and the concentration of the surfactant (cetyltrimethylammonium bromide, CTAB). Water contact angle measurements showed that the hydrophobicity of the prepared porous structures could be tuned by changing the pore size and wall thickness.

We demonstrate here that the electrochemical generation of hydroxyl ions and hydrogen bubbles can be used to induce the synthesis of enzyme- or protein-encapsulated 3D porous silica structure on the surface of noble metal electrodes. In the present work, the one-step synthesis of a glucose oxidase (GOD)-encapsulated silica matrix on a platinum electrode is presented. In this process, glucose oxidase was mixed with ethanol and TEOS to form a doped precursory sol solution. The electrochemically generated hydrogen bubbles at negative potentials assisted the formation of the porous structure of a GOD-encapsulated silica gel, and then the one-step immobilization of enzyme into the silica matrix was achieved. Scanning electron microscopy (SEM) and scanning electrochemical microscopy (SECM) characterizations showed that the GOD-encapsulated silica matrix adhered to the electrode surface effectively and had an interconnected porous structure. Because the pores started at the electrode surface, their sizes increased gradually along the distance away from the electrode and reached maximum at the solution side, and effective mass transport to the electrode surface could be achieved. The entrapped enzyme in the silica matrix retained its activity. The present glucose biosensor had a short response time of 2 s and showed a linear response to glucose from 0 to 10 mM with a correlation coefficient of 0.9932. The detection limit was estimated to be 0.01 mM at a signal-to-noise ratio of 3. The apparent Michaelis-Menten constant (K m app) and the maximum current density were determined to be 20.3 mM and 112.4 microA cm-2, respectively. The present method offers a facile way to fabricate biosensors and bioelectronic devices in situ.

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Adsorption of horseradish peroxidase (HRP) on graphite rod electrodes sequentially modified with carbon microfibers (CMF) carrying carbon nanotubes in a hierarchically structured arrangement and finally pyrene hexanoic acid (PHA) for improving hydrophilicity of the electrode surface is the basis for the direct bioelectrocatalytic reduction of H(2)O(2) at potentials as high as about +600 mV. The high-potential direct bioelectrocatalytic reduction of H(2)O(2) is implying a direct bioelectrochemical communication between the Fe(IV)=O,P(+*) redox state known as compound I. The HRP loading was optimized leading to a current of 800 microA at a potential of 300 mV.