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Characterization of faujasite-type zeolites with different Si/Al ratios using 29Si (27Al)Trapdor NMR
(2015)
One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4).
In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure.
One-part geopolymers, synthesized from three different silica sources and sodium aluminate, were investigated regarding their microstructure and the evolution of their compressive strength on curing at slightly elevated temperatures. The effect of thermal treatment was studied up to 1000 °C and for the investigation of the chemical durability specific samples were treated with sulfuric acid (H2SO4, pH = 1).
Depending on the silica feedstock, different degrees of reaction were observed. One of the silicas had a significantly higher reactivity. For two of the silicas, significant amounts of zeolites occurred as reaction products besides geopolymeric gel, whereas the more reactive silica source lead to the formation of a rather fully condensed geopolymeric network.
The composites indicated promising behavior on heating in so far as no distinct shrinkage step occurred in the temperature range of dehydration. Up to 400 °C the residual strength of those mixes increased. Above 800 °C the samples underwent new phase formation. After exposure to sulfuric acid (pH 1; 70 d) specimens showed a residual compressive strength of about 77 % of the reference, indicating high acid resistance.