New polyhedral oligomeric silsesquioxanes (POSS), ((BuSi)-Bu-i)(7)O12SiOSi(Me)(2)CH2(CH2)(n)CH2OC(O)C(CH3)=CH2 bearing one single methacrylate group, were synthesized by hydrosilylation of allylalcohol or 4-penten-1-ol, followed by acylation with methacryloyl chloride. All intermediates and final derivatives were carefully characterized by FTIR, H-1, C-13, and Si-29 solution state NMR, size exclusion chromatography (SEC), MALDI-TOF MS, and powder XRD (including full indexation of the diffraction patterns). In a second step, POSS/methacrylate based films were prepared. For 10 wt % of POSS, phase separation occurs with concomitant POSS crystallization. This behavior is not observed for 2 wt %, but XPS analyses show migration of POSS toward the film-air interface, which led to improved hydrophobic properties of the UV polymerized films with a 30 degrees increase in contact angle.
New Monofunctional POSS and Its Utilization as Dewetting Additive in Methacrylate Based Free-Standing Films / Mammeri, F., Bonhomme, C., Ribot, F., Babonneau, F., Dirè, S.. - In: CHEMISTRY OF MATERIALS. - ISSN 0897-4756. - 21:18(2009), pp. 4163-4171. [10.1021/CM900339H]
New Monofunctional POSS and Its Utilization as Dewetting Additive in Methacrylate Based Free-Standing Films
Dirè, Sandra
2009-01-01
Abstract
New polyhedral oligomeric silsesquioxanes (POSS), ((BuSi)-Bu-i)(7)O12SiOSi(Me)(2)CH2(CH2)(n)CH2OC(O)C(CH3)=CH2 bearing one single methacrylate group, were synthesized by hydrosilylation of allylalcohol or 4-penten-1-ol, followed by acylation with methacryloyl chloride. All intermediates and final derivatives were carefully characterized by FTIR, H-1, C-13, and Si-29 solution state NMR, size exclusion chromatography (SEC), MALDI-TOF MS, and powder XRD (including full indexation of the diffraction patterns). In a second step, POSS/methacrylate based films were prepared. For 10 wt % of POSS, phase separation occurs with concomitant POSS crystallization. This behavior is not observed for 2 wt %, but XPS analyses show migration of POSS toward the film-air interface, which led to improved hydrophobic properties of the UV polymerized films with a 30 degrees increase in contact angle.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione
