Citation
Foster, R. N.; Johansson, P. K.; Tom, N. R.; Koelsch, P.; & Castner, D. G. (2015). Experimental design and analysis of activators regenerated by electron transfer-atom transfer radical polymerization experimental conditions for grafting sodium styrene sulfonate from titanium substrates. J Vac Sci Technol A, 33(5), 05E131. PMCID: 4570287Abstract
A 24 factorial design was used to optimize the activators regenerated by electron transfer-atom transfer radical polymerization (ARGET-ATRP) grafting of sodium styrene sulfonate (NaSS) films from trichlorosilane/10-undecen-1-yl 2-bromo-2-methylpropionate (ester ClSi) functionalized titanium substrates. The process variables explored were: (1) ATRP initiator surface functionalization reaction time; (2) grafting reaction time; (3) CuBr2 concentration; and (4) reducing agent (vitamin C) concentration. All samples were characterized using x-ray photoelectron spectroscopy (XPS). Two statistical methods were used to analyze the results: (1) analysis of variance with [Formula: see text], using average [Formula: see text] XPS atomic percent as the response; and (2) principal component analysis using a peak list compiled from all the XPS composition results. Through this analysis combined with follow-up studies, the following conclusions are reached: (1) ATRP-initiator surface functionalization reaction times have no discernable effect on NaSS film quality; (2) minimum (=24 h for this system) grafting reaction times should be used on titanium substrates since NaSS film quality decreased and variability increased with increasing reaction times; (3) minimum (=0.5 mg cm-2 for this system) CuBr2 concentrations should be used to graft thicker NaSS films; and (4) no deleterious effects were detected with increasing vitamin C concentration.Notes
Foster, Rami NJohansson, Patrik K
Tom, Nicole R
Koelsch, Patrick
Castner, David G
P41 EB002027/EB/NIBIB NIH HHS/
J Vac Sci Technol A. 2015 Sep;33(5):05E131. Epub 2015 Aug 27.
