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21.For the in-beam experiments and Cl-free electrolyte, only one field of view is available per datapoint. The number of clusters is divided by the imaged area, with an error bar equal to the square root of the number of clusters divided by the area of the image, in accordance with an assumption that the number of clusters per area follows a Poisson distribution. As the overpotential increases, the growth rate increases leading to rapid coalescence. A movie frame is chosen from a slightly earlier time to resolve clusters before coalescence and allow more accurate measurement of density. At −130 mV the clusters are too close to distinguish and we show only a lower bound. For the out of beam data points, the movie taken during the survey around the electrode is cut into non-overlapping images. For 6 of the 11 experiments we have at least two such images available and the density among these images appears consistent. The datapoint is the average and the error bars represent the maximum and minimum density observed. If no clusters are found, the upper limit is calculated as 1/total area inspected. For the other 5 of the 11 experiments the cluster density varies widely: the datapoint represents an estimate of the density and the error bars represent an estimate of the confidence interval.
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40.The mechanism has some analogies with the reduction of AgCl to Ag metal by photons when exposing photographic plates. This poses the question of whether visible illumination affects deposition in a Cl -containing electrolyte. CV and current-time transients in the Cl-containing electrolyte showed small effects when switching a 500 W halogen lamp light source on and off. However, by changing the timing of the illumination, these effects appeared to be due to temperature changes via lamp heating. We cannot rule out effects at higher intensity.
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We describe a technique for patterning clusters of metal using electrochemical deposition. By operating an electrochemical cell in the transmission electron microscope, we deposit Cu on Au under potentiostatic conditions. For acidified copper sulphate electrolytes, nucleation occurs uniformly over the electrode. However, when chloride ions are added there is a range of applied potentials over which nucleation occurs only in areas irradiated by the electron beam. By scanning the beam we control nucleation to form patterns of deposited copper. We discuss the mechanism for this effect in terms of electron beam-induced reactions with copper chloride, and consider possible applications.


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