Abstract
Silanols and silanes are key precursors and intermediates for the synthesis of silicon‐based materials. While their characterization and quantification by 29Si NMR spectroscopy has received significant attention, it is a technique that is limited by the low natural abundance of 29Si and its low sensitivity. Here, we describe a method using p‐H2 to hyperpolarize 29Si. The observed signal enhancements, approaching 3000‐fold at 11.7 T, would take many days of measurement for comparable results under Boltzmann conditions. The resulting signals were exploited to monitor the rapid reaction of tris(tert‐butoxy)silanol with triflic anhydride in a T 1‐corrected process that allows for rapid quantification. These results demonstrate a novel route to quantify dynamic processes and intermediates in the synthesis of silicon materials.
Highlights
We develop the SABRE-Relay technique for the hyperpolarization of silanols by p-H2 and direct silane polarization by SABRE
Of it's three naturally occurring isotopes, only 29Si has a non-zero magnetic moment and its nuclear magnetic resonance (NMR) detection is of wide interest
29Si NMR spectroscopy has limitations that reduce its potential use,[2] primarily due to its low sensitivity that is dependent upon the small population differences that exist between nuclear spin energy levels within a magnetic field
Summary
After SABRE-Relay transfer, an improved silanol signal gain of 92±4-fold was observed (Figure 1B). Signal gains could be increased if the SABRE-Relay time was extended beyond 10 s.
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