The sol–gel process is an effective method for
the preparation
of homogeneous structured nanomaterials whose physico-chemical properties
strongly depend on the experimental conditions applied. The control
of a three-component reaction with silanes showing multiple reaction
sites revealed the need for an analytical tool that allows a rapid
response to ongoing transformations in the reaction mixture. Herein,
we describe the implementation of near-infrared (NIR) spectroscopy
based on compact, mechanically robust, and cost-efficient micro-optomechanical
system technology in the sol–gel process of three silanes with
a total of nine reaction sites. The NIR-spectroscopically controlled
reaction yields a long-time stable product with reproducible quality,
fulfilling the demanding requirements for further use in coating processes.1H nuclear magnetic resonance measurements are used as reference
values for the calibration of a partial least squares (PLS) regression
model. The precise prediction of the desired parameters from collected
NIR spectroscopy data acquired during the sol–gel reaction
proves the applicability of the calibrated PLS regression model. The
determined shelf-life and further processing tests verify the high
quality of the sol–gel and the produced highly cross-linked
polysilane.