Sequential Infiltration Synthesis of Al2O3in Biodegradable Polybutylene Succinate: Characterization of the Infiltration Mechanism

Year: 2022

Authors: Motta A., Seguini G., Perego M., Consonni R., Boccia A.C., Ambrosio G., Baratto C., Cerruti P., Lavorgna M., Tagliabue S., Wiemer C.

Autors Affiliation: CNR IMM, Unit Agrate Brianza, I-20864 Agrate Brianza, Italy; Politecn Milan, Dept Energy, I-20133 Milan, Italy; CNR SCITEC, I-20133 Milan, Italy; CNR INO, PRISM Lab, I-25123 Brescia, Italy; CNR IPCB, I-23900 Lecce, Italy; Corapack srl, I-22040 Brenna, Italy.

Abstract: The introduction of inorganic materials into biopol-ymers has been envisioned as a viable option to modify the optical and structural properties of these polymers and promote their exploitation in different application fields. In this work, the growth of Al2O3 in freestanding similar to 30-mu m-thick poly(butylene succinate) (PBS) films by sequential infiltration (SIS) at 70 degrees C via trimethylaluminum (TMA) and H2O precursors was investigated for the first time. The incorporation of Al2O3 into the PBS matrix was clearly demonstrated by XPS analysis and SEM-EDX cross-sectional images showing a homogeneous Al2O3 distribution inside the PBS films. Raman measurements on infiltrated freestanding PBS show a reduction of the signal related to the ester carbonyl group as compared to pristine freestanding PBS films. Accordingly, FTIR and NMR characterization highlighted that the ester group is involved in polymer-precursor interaction, leading to the formation of an aliphatic group and the concomitant rupture of the main polymeric chain. Al2O3 mass uptake as a function of the number of SIS cycles was studied by infiltration in thin PBS films spin-coated on Si substrates ranging from 30 to 70 nm. Mass uptake in the PBS films was found to be much higher than in standard poly(methyl methacrylate) (PMMA) films, under the same process conditions. Considering that the density of reactive sites in the two polymers is roughly the same, the observed difference in Al2O3 mass uptake is explained based on the different free volume of these polymers and the specific reaction mechanism proposed for PBS. These results assessed the possibility to use SIS as a tool for the growth of metal oxides into biopolymers, paving the way to the synthesis of organic-inorganic hybrid materials with tailored characteristics.

Journal/Review: ACS APPLIED POLYMER MATERIALS

Volume: 4 (10)      Pages from: 7191  to: 7203

More Information: The authors would like to thank Eleonora Bonaventura (CNR-IMM, Unit of Agrate Brianza) who help the authors in acquiring UV-vis spectra. This research was supported by the project “sPATIALS3”, financed by the European Regional Development Fund under the ROP of the Lombardy Region ERDF 2014-2020-Axis I “Strengthen technological research, development and innovation”-Action 1.b.1.3 “Support for co-operative R & D activities to develop new sustainable technologies, products and services”-Call Hub.
KeyWords: biopolymers, hybrid materials, Al2O3, TMA, SIS, packaging, NM36277172R, spectroscopy
DOI: 10.1021/acsapm.2c01073

Citations: 5
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