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High-throughput biological assays were used to develop structure - antimicrobial relationships for polysiloxane coatings containing chemically bound (tethered) quaternary ammonium salt (QAS) moieties. The QAS-functional polysiloxanes were derived from solution blends of a silanol-terminated polydimethylsiloxane, a trimethoxysilane-functional QAS (QAS-TMS), and methylacetoxysilane. Since the QAS moieties provide antimicrobial activity through interaction with the microorganism cell wall, most of the compositional variables that were investigated were associated with the chemical structure of the QAS-TMS. Twenty different QAS-TMS were synthesized for the study and the antimicrobial activity of sixty unique polysiloxane coatings derived from these QAS-TMS determined toward Escherichia coli , Staphylococcus aureus , and Candida albicans . The results of the study showed that essentially all of the compositional variables significantly influenced antimicrobial activity. Surface characterization of these moisture-cured coatings using atomic force microscopy as well as water contact angle and water contact angle hysteresis measurements indicated that the compositional variables significantly affected coating surface morphology and surface chemistry. Overall, compositional variables that produced heterogeneous surface morphologies provided the highest antimicrobial activity suggesting that the antimicrobial activity was primarily derived from the relationship between coating chemical composition and self-assembly of QAS moieties at the coating/air interface. Using data modeling software, a narrow region of the compositional space was identified that provided broad-spectrum antimicrobial activity.

An automated, high-throughput adhesion workflow that enables pseudobarnacle adhesion and coating/substrate adhesion to be measured on coating patches arranged in an array format on 4x8 in.(2) panels was developed. The adhesion workflow consists of the following process steps: (1) application of an adhesive to the coating array; (2) insertion of panels into a clamping device; (3) insertion of aluminum studs into the clamping device and onto coating surfaces, aligned with the adhesive; (4) curing of the adhesive; and (5) automated removal of the aluminum studs. Validation experiments comparing data generated using the automated, high-throughput workflow to data obtained using conventional, manual methods showed that the automated system allows for accurate ranking of relative coating adhesion performance.

An array of quaternary ammonium functionalized-polyhedral oligomeric silsesquioxane (Q-POSS) compounds with different alkyl chain lengths and counter ions were synthesized using a two-step process. First, octasilane POSS was functionalized with dimethylamino groups by hydrosilylation with allyldimethylamine. Next, partial quaternization of the tertiaryamino-functional POSS was achieved using an alkyl halide to produce the Q-POSS. Alkyl chain length of the Q-POSS compounds varied from -C 12 H 25 to -C 18 H 37 and the counter ions varied between chlorine, bromine, and iodine. Moisture-cured polysiloxane coatings were prepared by dispersing Q-POSS molecules into a solution blend of silanol-terminated polydimethylsiloxane, methylacetoxysilane, and a catalyst. To evaluate the utility of the Q-POSS molecules as a broad-spectrum antimicrobial additive, the antimicrobial activity of the coatings toward the Gram-negative bacterium, Escherichia coli, the Gram-positive bacterium, Staphylococcus aureus, and the opportunistic fungal pathogen, Candida albicans, was determined using an agar plating method. The results obtained showed that both the composition of the Q-POSS and the composition of the polysiloxane matrix affected antimicrobial properties. Compositions were identified that inhibited the growth of all three microorganisms on the coating surface. Surface Raman spectroscopic analysis was performed on selected set of coatings to understand the relative concentration of Q-POSS molecules at the coating surface.

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