The objective of this experimental work was to study the rheological behavior of blends composed of unsaturated polyester resin and calcium carbonate. The influence of calcium carbonate content on the viscosity of the resin has been first investigated for calcium carbonate contents ranging from 0 to 60 wt%. Furthermore, the influences of shear rate and standing time have also been analyzed for different resin/fillers blends. The experimental results show a complex rheological behavior, and allow us to better control the composite formulation as a function of the required molding characteristics and properties of the final composite.
Alkoxysilanes, and mainly trialkoxysilanes, have been widely used as coupling agents on metallic surfaces. They are of interest mainly because they form a water-stable covalent bond with a surface composed of hydroxides. The grafting of these molecules should also give rise to the formation of a siloxane network at the substrate's surface. However, only a few studies examine stainless steel substrate, such as AISI 316L, for which the main difficulty is the low surface reactivity. In order to improve the silane anchoring, a prehydrolysis of the alkoxysilane was performed to transform the methoxy groups into silanol groups. This reaction happened in an aqueous medium and at a controlled pH, which impacted the prehydrolysis efficiency. Curing followed this step, which allows the grafting of the alkoxysilane on stainless steel's surface. Polarization modulation infrared reflection absorption spectroscopy (PM-IRRAS) was performed in order to identify the grafting of the silane molecules. Tests were made to compare the grafting of alkoxysilanes as a function of their functional groups and their prehydrolysis conditions. PM-IRRAS coupled with atomic force microscopy allowed the observation of the grafting of the studied alkoxysilanes. The nature of the remaining functional group (its ability to react with polymer, for example) of the alkoxysilane plays a major role in this process, since its chemical nature influences the grafting mechanism.
The grafting of trialkoxysilane molecules should also give rise to the formation of a siloxane network at the substrate's surface when trialkoxysilanes are used. Other candidates that might be able to act as adhesion promoters at metallic surfaces are dimethylalkoxysilanes. The advantage of dimethylalkoxysilanes is that only one silanol group is produced during the hydrolysis step, leading to the formation of a grafted monolayer onto the steel. Moreover, the chemical grafting of stainless steel, which exhibits a low surface reactivity, is of great interest for industrial applications such as adhesive bonding or coatings. The objective of this work was to chemically graft dimethylalkoxysilanes onto AISI 316L stainless steel and to analyze the grafted layer by X‐ray photoelectron spectroscopy (XPS). Investigation of the hydrolysis of these molecules in aqueous solutions was also performed by proton nuclear magnetic resonance spectroscopy (1H NMR). The grafting of 3‐(ethoxydimethylsilyl)propylamine (APDES) and 3‐glycidoxypropyldimethylethoxysilane (GPDES) was achieved onto stainless steel after a controlled hydrolysis reaction. A pH inferior or equal to 5 was necessary to obtain a sufficient hydrolysis of silanes. XPS results have evidenced the grafting of the silanes onto stainless steel. The signal of the Si 2p peak clearly showed the formation of a covalent bond between APDES and the stainless steel surface through the O atoms giving rise to a uniform layer of adsorbed molecules. Moreover, this grafted layer is strongly stable as no removal of the alkoxysilane was observed after immersion in hot water which is very critical for these molecules. Copyright © 2015 John Wiley & Sons, Ltd.
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