Characterization of self-assembled Bis[2-(2-bromoisobutyryloxy) undecyl] disulphide (DTBU) on gold surfaces suitable for use in surface-initiated atom transfer radical polymerization (SI-ATRP)
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Author
Chávez, Miriam
Fuentes-Rodríguez, Laura
Sánchez-Obrero, Guadalupe
Madueño, Rafael
Sevilla, José Manuel
Blázquez, Manuel
Pineda, Teresa
Publisher
ElsevierDate
2022Subject
DTBU radical polymerization initiatorSelf-assembled monolayer
6-Mercaptopurine 6MP
Mixed monolayers
Cyclic voltammetry
Electrochemical impedance spectroscopy
Contact angle
XPS
IRRAS
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Show full item recordAbstract
Bis[2-(2-bromoisobutyryloxy) undecyl] disulphide (DTBU) is an initiator for surface-initiated atom transfer
radical polymerization (SI-ATRP) able to functionalize metal surfaces through formation of self-assembled
monolayers (SAM). The goal of this work is the making monolayers with the DTBU initiator on gold polycrystalline
electrodes and their study by electrochemical methods as cyclic voltammetry (CV), capacity-potential
curves (C-E), electrochemical impedance spectroscopy (EIS), and angle contact measurements for their characterization.
Information of the integrity and permeability of the monolayers has been obtained by capacitancepotential
measurements and impedance spectra. Also, the blocking effect of the physical barrier that SAM can
produce to different redox probes is explored by using voltammetry and impedance. DTBU forms a compact
monolayer whose main features are related with heterogeneous chain structures, having a non-polar hydrocarbon
internal part and a polar head group. This is confirmed by X-ray photoelectron spectroscopy (XPS) which
shows the presence of the elements of the DTBU adsorbate of SAM. Moreover, mixed monolayers of DTBU and
6-mercaptopurine (6MP) have been prepared and characterized, to check if the thiol facilitates electron
exchange through monolayers. On this approach, different DTBU:6MP ratios have been employed and characterized
studying IRRAS spectra, electrochemical properties, and contact angle on the modified surface. These
mixed monolayers provide optimal conditions for adaptation and use in e-ATRP.