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Archeological wood conservation with selected organosilicon compounds studied by XFM and nanoindentation

2023, Broda, Magdalena, Jakes, Joseph E., Li, Luxi, Antipova, Olga A.

AbstractWaterlogged wood conservation is a complex and challenging task. Detailed knowledge about the interactions between the applied chemicals and wood is necessary to ensure the effective and safe conservation of wooden artifacts. The present research aims to determine the mechanism of dimensional stabilization of archeological wood by organosilicon compounds using the combination of synchrotron-based X-ray fluorescence microscopy (XFM) and nanoindentation. Archeological oak wood was treated with methyltrimethoxysilane, (3-mercaptopropyl)trimethoxysilane, or 1,3-bis-[(diethylamino)-3-(propoxy)propan-2-ol]-1,1,3,3-tetramethyldisiloxane, which in previous studies were found to be more effective than other organosilicons in stabilizing wood dimensions. The XFM and nanoindentation results showed that all three organosilicons infiltrated wood cell walls and enhanced their mechanical properties. The XFM also showed that part of the chemicals filled some void spaces like cell lumina. Based on the results obtained here and in our previous research, it is determined that the mechanism of archeological wood dimensional stabilization by organosilicon treatment is complex and likely involves both filling cell lumina and infiltration into cell walls where organosilicons interact with wood polymers.

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Conservation of model degraded pine wood with selected organosilicons studied by XFM and nanoindentation

2024, Broda, Magdalena, Jakes, Joseph E., Li, Luxi, Antipova, Olga A., Maxey, Evan R., Jin, Qiaoling, Uniwersytet Przyrodniczy w Poznaniu, Forest Products Laboratory, Advanced Photon Source, Argonne National Laboratory

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Nanocellulose-Based Films for Surface Protection of Wooden Artefacts

2024, Kryg Paulina, Mazela, Bartłomiej, Perdoch, Waldemar, Jancelewicz Mariusz, Broda, Magdalena

This research investigated the selected properties of nanocellulose films intended to serve as protective patches on fissured surfaces of wooden artefacts. The effects of their plasticisation with glycerol and functionalisation with selected silanes ((3-Glycidyloxypropyl)trimethoxysilane, and Methyltrimethoxysilane) were also determined. The obtained pure cellulose nanopapers (CNPs) had a homogeneous and compact structure but were very brittle, stiff, and wavy. Functionalisation with silanes made their structure more packed and reduced their equilibrium moisture content by 87–96%, depending on the type and concentration of the silane. Silane functionalisation also slightly improved nanopapers’ resistance to moulds. Plasticisation with glycerol provided CNPs with higher flexibility and resistance to fracture and made them flatter and smoother, reducing the wettability of their surfaces but increasing their hygroscopicity (EMC values increased 1.7–3.5 times for pure CNPs and 5–33 times for functionalised CNPs) and vulnerability to mould infestation. All prepared nanopapers can be easily glued to the wood surface and colour-matched using a nitro wood stain, oil paint or waterborne acrylic paint. The research showed that cellulose nanopapers modified with silanes and plasticised with glycerol seem to be a promising solution for protecting the cracked surface of wooden artefacts against further degradation due to external conditions.

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Reactivity of Waterlogged Archeological Elm Wood with Organosilicon Compounds Applied as Wood Consolidants: 2D 1H–13C Solution-State NMR Studies

2022, Broda, Magdalena, Yelle, Daniel J.

Some organosilicon compounds, including alkoxysilanes and siloxanes, proved effective in stabilizing the dimensions of waterlogged archaeological wood during drying, which is essential in the conservation process of ancient artifacts. However, it was difficult to determine a strong correlation between the wood stabilizing effect and the properties of organosilicon compounds, such as molecular weight and size, weight percent gain, and the presence of other potentially reactive groups. Therefore, to better understand the mechanism behind the stabilization effectiveness, the reactivity of organosilicons with wood polymers was studied using a 2D 1H–13C solution-state NMR technique. The results showed an extensive modification of lignin through its demethoxylation and decarbonylation and also the absence of the native cellulose anomeric peak in siloxane-treated wood. The most substantial reactivity between wood polymers and organosilicon was observed with the (3-mercaptopropyl)trimethoxysilane treatment, showing complete removal of lignin side chains, the lowest syringyl/guaiacyl ratio, depolymerization of cellulose and xylan, and reactivity with the C6 primary hydroxyls in cellulose. This may explain the outstanding stabilizing effectiveness of this silane and supports the conclusion that extensive chemical interactions are essential in this process. It also indicates the vital role of a mercapto group in wood stabilization by organosilicons. This 2D NMR technique sheds new light on the chemical mechanisms involved in organosilicon consolidation of wood and reveals what chemical characteristics are essential in developing future conservation treatments.