Electrosynthesis and electrodoping of C[sub 60][sup n[minus]] (n = 0, 1, 2, or 3) films. Electrochemical quartz crystal microbalance study in acetonitrile solutions of alkali-metal, alkaline-earth-metal, and tetra-n-butylammonium cations

Journal Article · Thu Jul 01 04:00:00 EDT 1993 · Journal of Physical Chemistry; (United States)

DOI:https://doi.org/10.1021/j100128a021· OSTI ID:5146726

Koh, W; Dubois, D; Kutner, W; Jones, M T; Kadish, K M ^[1]

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1. Univ. of Houston, TX (United States)

The electrosynthesis, electrodoping/undoping, and electrodissolution of thin films of C[sub 60] and its salts were studied in acetonitrile solutions at a Au/quartz electrode by simultaneous electrochemistry and microgravimetry with an electrochemical quartz crystal microbalance. The C[sub 60][sup 0] films were deposited either by electrooxidation of C[sub 60][sup 2[minus]] in solutions containing CsAsF[sub 6], KPF[sub 6], or Ca(PF[sub 6])[sub 2], or by electrooxidation of C[sub 60][sup 3[minus]] in solutions containing tetra-n-butylammonium perchlorate, (TBA)ClO[sub 4]. The initial C[sub 60][sup 2[minus]] or C[sub 60][sup 3[minus]] anions were prepared by controlled-potential bulk electroreduction of a C[sub 60][sup 0] suspension. The C[sub 60][sup 0] films electrodeposited from a C[sub 60][sup 2[minus]] solution containing Cs[sup +], K[sup +], or Ca[sup 2+] cations could not be electrodoped with these cations but a conductive (Cs[sup +])[sub 3](C[sub 60][sup 3[minus]]) film could be quantitatively electrosynthesized by electroreduction of C[sub 60][sup 2[minus]] in a solution containing Cs[sup +]. Attempts to electrodeposit (K[sup +])[sub 3](C[sub 60][sup 3[minus]]) or (Ca[sup 2+])[sub 3](C[sub 60][sup 3[minus]])[sub 2] films were successful but a (Ca[sup 2+])(C[sub 60][sup [minus]])[sub 2] film could be prepared. The composition of a given C[sub 60][sup 0] film electrodeposited by constant potential electrooxidation of C[sub 60][sup 3[minus]] in an acetonitrile solution containing (TBA)ClO[sub 4] was controlled by the initial C[sub 60][sup 3[minus]] concentration and/or the electrodeposition potential. These C[sub 60][sup 0] films could be electrodoped with TBA[sup +] cations from solution upon electroreduction at appropriate potentials and both (TBA[sup +])(C[sub 60][sup [minus]]) and (TBA[sup +])[sub 2](C[sub 60][sup 2[minus]]) films were obtained. 66 refs., 10 figs.

• OSTI ID: 5146726
• Journal Information: Journal of Physical Chemistry; (United States), Journal Name: Journal of Physical Chemistry; (United States) Vol. 97:26; ISSN JPCHAX; ISSN 0022-3654
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
400400 -- Electrochemistry
ACETONITRILE
ALKALI METAL COMPOUNDS
ALKALINE EARTH METAL COMPOUNDS
AMINES
AMMONIUM COMPOUNDS
BALANCES
CARBON
CHEMISTRY
CRYSTAL DOPING
DISPERSIONS
ELECTROCHEMISTRY
ELEMENTS
FILMS
FULLERENES
MEASURING INSTRUMENTS
MICROBALANCES
MIXTURES
NITRILES
NONMETALS
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
QUATERNARY COMPOUNDS
SALTS
SOLUTIONS
SYNTHESIS
THIN FILMS
WEIGHT INDICATORS