XPS Study on the Use of 3-Aminopropyltriethoxysilane to Bond Chitosan to a Titanium Surface

Abstract

Chitosan, a biopolymer found in the exoskeletons of shellfish, has been shown to be antibacterial, biodegradable, osteoconductive, and has the ability to promote organized bone formation. These properties make chitosan an ideal material for use as a bioactive coating on medical implant materials. In this study, coatings made from 86.4% de-acetylated chitosan were bound to implant-quality titanium. The chitosan films were bound through a three-step process that involved the deposition of 3-aminopropyltriethoxysilane (APTES) in toluene, followed by a reaction between the amine end of APTES with gluteraldehyde, and finally, a reaction between the aldehyde end of gluteraldehyde and chitosan. Two different metal treatments were examined to determine if major differences in the ability to bind chitosan could be seen. X-ray photoelectron spectroscopy (XPS) was used to examine the surface of the titanium metal and to study the individual reaction steps. The changes to the titanium surface were consistent with the anticipated reaction steps, with significant changes in the amounts of nitrogen, silicon, and titanium that were present. It was demonstrated that more APTES was bound to the piranha-treated titanium surface as compared to the passivated titanium surface, based on the amounts of titanium, carbon, nitrogen, and silicon that were present. The metal treatments did not affect the chemistry of the chitosan films. Using toluene to bond APTES on titanium surfaces, rather than aqueous solutions, prevented the formation of unwanted polysiloxanes and increased the amount of silane on the surface for forming bonds to the chitosan films. Qualitatively, the films were more strongly attached to the titanium surfaces after using toluene, which could withstand the ultrahigh vacuum environment of XPS, as compared to the aqueous solutions, which were removed from the titanium surface when exposed to the ultrahigh vacuum environment of XPS.

Grafting of antibacterial polymers on stainless steel via surface‐initiated atom transfer radical polymerization for inhibiting biocorrosion by Desulfovibrio desulfuricans

“…The wide scan spectrum of the oxidized/hydroxylated (SS-OH) surface, from the piranha solution treatment (Martin et al, 2007;Yuan et al, 2008), is dominated by Fe 2p, Cr 2p, O 1s and C 1s signals (Fig. 2a).…”

“…The grease-free and smooth coupons were treated by Piranha solution to generate a hydroxyl-enriched (SS-OH), or a hydroxylated surface. Details on the preparation and characterization of the hydroxylated surface had been described previously (Martin et al, 2007;Yuan et al, 2008). The silane coupling agent, CTS, was immobilized on the hydroxylated substrate via self-assembly.…”

“…Well-defined and dense polymer brushes covalently bonded to a metal surface can render excellent mechanical and chemical protection to the substrate, alter the electrochemical characteristics of the interface, and provide versatility in coating formulation (Fan et al, 2005;Fu et al, 2005;Martin et al, 2007).…”

Morphology and Amine Accessibility of (3‐Aminopropyl) Triethoxysilane Films on Glass Surfaces

“…Silanization of solid surfaces with APTES is widely used to prepare substrates for applications using immobilized proteins and to prepare selective absorbents or organic/inorganic hybrid materials (Kurth and Bein, 1995;Hu et al ., 1996;Frey et al ., 1997;Joos et al ., 1997;Szabo et al ., 1998;Gyorvary et al ., 1999;Falsey et al ., 2001;LeProust et al ., 2001;Kim and Abbott, 2002;Matsumoto et al ., 2002;Ek et al ., 2003;Etienne and Walcarius, 2003;Jin et al ., 2003;Miyazaki et al ., 2003;Vaidya and Norton, 2004;Crampton et al ., 2005;Chen et al ., 2006;Enders et al ., 2007;Martin et al ., 2007;Yu et al ., 2007). Chemically adsorbed silane on an inorganic surface provides a platform for further chemical reactions through an amine or other functional group opposite to the silane.…”

Study on the use of 3‐aminopropyltriethoxysilane and 3‐chloropropyltriethoxysilane to surface biochemical modification of a novel low elastic modulus Ti–Nb–Hf alloy

“…This problem can be overcome, at least in part, by adding a preliminary activation treatment. For pure titanium, there is a large diversity of examples in the literature suggesting different activation methods to provide reactive groups for covalent immobilization of biomolecules (mainly -OH groups) [2][3][4][5][6][7][8][9][10][11] and organosilanes bearing different functional groups [12][13][14][15][16][17]. Recently, a comparative study between two activation methods frequently used (Oxygen plasma and Piranha solution) was performed by V. Paredes [18].…”