Chemical reactions of electrochemically reduced fullerene and combining scanning electrochemical microscopy with other analytical methods

The chemical reactions of electrochemically generated fullerene anions with protons and when complexed to t-butylcalix (8) arene are studied. First, electrochemical studies of the protonation reactions of the monoanion and dianion of C{dollar}sb{lcub}60{rcub}{dollar} were carried out in acetonitrile and o-dichlorobenzene. These studies also used near-infrared spectrometry and mass spectroscopy to confirm the electrochemical results. The results show that the monoanion is a very weak base, but the dianion is more basic. Studies of C{dollar}sb{lcub}60{rcub}{dollar} and t-butylcalixarene/C{dollar}sb{lcub}60{rcub}{dollar} films using the electroanalytical methods of scanning electrochemical microscopy (SECM) and quartz crystal microbalance (QCM) show the anions of C{dollar}sb{lcub}60{rcub}{dollar} dissolve in acetonitrile to various degrees depending on supporting electrolyte.; The other aspect of the work is the creation of combining other electroanalytical techniques to an existing scanning electrochemical microscope. The combination of SECM with a QCM is used for studying silver and C{dollar}sb{lcub}60{rcub}{dollar} films, and the fundamental mechanics of combining the two is discussed. The combination of SECM with electrogenerated chemiluminescence (ECL) to perform scanning electrochemical luminescence microscopy (SECLM), a new scanning probe microscopy, is demonstrated and preliminary images are presented for a number of ECL reaction systems. The final combination explores the ability to combine SECM with near-field scanning optical microscopy (NSOM). The issues of NSOM tip construction and creation of an electrode on the NSOM tip are discussed with a variety of experiments detailing the attempts.