Sequential Infiltration Synthesis of Silicon Dioxide in Polymers with Ester Groups–Insight from In Situ Infrared Spectroscopy

Biswas, Mahua; Rozyyev, Vepa; Mane, Anil U.; Korveziroska, Amelia; Manna, Uttam; Elam, Jeffrey W.

doi:10.1021/acs.jpcc.3c07571

Title: Sequential Infiltration Synthesis of Silicon Dioxide in Polymers with Ester Groups–Insight from In Situ Infrared Spectroscopy

Journal Article · 03 April 2024 · Journal of Physical Chemistry. C

DOI: https://doi.org/10.1021/acs.jpcc.3c07571 · OSTI ID:2333075

^[1]; Rozyyev, Vepa ^[2]; Mane, Anil U. ^[3]; Korveziroska, Amelia ^[1];

^[1];

^[3]

Illinois State University (ISU), Normal, IL (United States)
Argonne National Laboratory (ANL), Argonne, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Advanced Materials for Energy-Water Systems (AMEWS); Univ. of Chicago, IL (United States)
Argonne National Laboratory (ANL), Argonne, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Advanced Materials for Energy-Water Systems (AMEWS)

New strategies to synthesize nanometer-scale silicon dioxide (SiO₂) patterns have drawn much attention in applications such as microelectronic and optoelectronic devices, membranes, and sensors, as we are approaching device dimensions shrinking below 10 nm. In this regard, sequential infiltration synthesis (SIS), a two-step gas-phase molecular assembly process that enables localized inorganic material growth in the targeted reactive domains of polymers, is an attractive process. In this work, we performed in situ Fourier transform infrared spectroscopy (FTIR) measurements during SiO₂ SIS to investigate the reaction mechanism of trimethylaluminum (TMA) and tri(tert-pentoxy) silanol (TPS) precursors with polymers having ester functional groups (poly(methyl methacrylate) (PMMA), poly(ethyl methacrylate) (PEMA), polycaprolactone (PCL), and poly(t-butyl methacrylate) (PBMA)), for the purpose of growing patterned nanomaterials. The FTIR results show that for PMMA and PEMA, a lower percentage of functional groups participated in the reactions and formed weak and unstable complexes. In contrast, almost all functional groups in PCL and PBMA participated in the reactions and showed stable and irreversible interactions with TMA. We discovered that the amount of SiO₂ formed is not directly correlated with the number of interacting functional groups. These insights into the SiO₂ SIS mechanism will enable nanopatterning of SiO₂ for low-dimensional applications.

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Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Advanced Materials for Energy-Water Systems (AMEWS)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF)

Grant/Contract Number:: AC02-06CH11357; DMR- 2213365

OSTI ID:: 2333075

Alternate ID(s):: OSTI ID: 2467335

Journal Information:: Journal of Physical Chemistry. C, Vol. 128, Issue 15; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Title: Sequential Infiltration Synthesis of Silicon Dioxide in Polymers with Ester Groups–Insight from In Situ Infrared Spectroscopy

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