Journal
LANGMUIR
Volume 39, Issue 23, Pages 8153-8162Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.langmuir.3c00601
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The sol-gel process is an effective method for preparing homogeneous structured nanomaterials, and its properties depend on experimental conditions. This study implemented near-infrared spectroscopy based on micro-optomechanical system technology in the sol-gel process of three silanes. The controlled reaction yielded a stable product with reproducible quality, fulfilling the requirements for coating processes.
The sol-gel process is an effective method forthe preparationof homogeneous structured nanomaterials whose physico-chemical propertiesstrongly depend on the experimental conditions applied. The controlof a three-component reaction with silanes showing multiple reactionsites revealed the need for an analytical tool that allows a rapidresponse to ongoing transformations in the reaction mixture. Herein,we describe the implementation of near-infrared (NIR) spectroscopybased on compact, mechanically robust, and cost-efficient micro-optomechanicalsystem technology in the sol-gel process of three silanes witha total of nine reaction sites. The NIR-spectroscopically controlledreaction yields a long-time stable product with reproducible quality,fulfilling the demanding requirements for further use in coating processes. H-1 nuclear magnetic resonance measurements are used as referencevalues for the calibration of a partial least squares (PLS) regressionmodel. The precise prediction of the desired parameters from collectedNIR spectroscopy data acquired during the sol-gel reactionproves the applicability of the calibrated PLS regression model. Thedetermined shelf-life and further processing tests verify the highquality of the sol-gel and the produced highly cross-linkedpolysilane.
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