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Untersuchung historischer Goldmosaike Herstellungstechnologie und charakteristische Schadensbilder
(2009)
Imprägnierung von Holz mit SiO2- und/oder SiO2-Solen: Fixierung der anorganischen Komponente im Holz
(2010)
The solgel process was applied to enhance properties of pine sapwood. For this purpose wood prisms were soaked in nanoscaled precursor solutions prepared from titanium(IV) n-butoxide and titanium(IV) iso-propoxide, respectively, using vacuum impregnation technique. The wet composites were cured by special program with final heat treatment at 103 °C. Weight percent gains (WPG) of the wood specimen in the range of 19-25% were obtained due to these procedures. SEM investigations show that precursor solutions penetrate into the whole wood body and the titania formed after heat treatment in the composites is deposited in the pores (lumen) and partly in the cell walls of the wooden matrix. The moisture sorption was investigated in long term tests for a period of some months by storage at 20-23 °C in humid air (relative humidity of 99%) and ambient atmosphere (relative humidity 40-60%), respectively. For untreated reference samples the moisture sorption results in increasing of mass and volume according to saturation values of 24 and 13%, respectively, after about 15 days. The incorporation of titania reduces the saturation values of the moisture sorption by up to 12% in mass and by up to 5% in volume at a relative humidity of 99%. Thus, an enhancement of the dimensional stability of about 60% is obtained at best. The results demonstrate that modification of wood with sol-gel derived precursors can enhance its dimensional stability, which prevents the formation of cracks. Because of that reduced moisture sorption biological attacks should be delimited. Additionally, thermal analyses show a retarded combustion of the wood matrix due to titania infiltration.
The present study contributes to the controversial discussion in the literature whether Si–O–C bonds in wood–silica–gel composites exist. 13C NMR is a suitable method to proof such bonds. Because of the low concentration of 13C isotopes in natural wood, 13C cellulose was used as 13C-enriched substitute. A tailored sol for the impregnation of that cellulose was chosen by liquid 29Si NMR pre-investigations of various sols whose reactivity and stability were time-dependently analysed. It is based on a sub-stoichiometric hydrolysis of tetraethoxysilane (TEOS) with 1 mol water per mol TEOS. Thermal analyses were performed to show a comparability of the thermal behaviour of wood–silica–gel and cellulose–silica–gel composites. There are two strong hints of the existence of stable Si–O–C bonds: (1) by thermal analysis, a shift in the fire behaviour of 100 K can be observed with a change in pyrolysis behaviour of the composite and (2) the proof by REDOR NMR that a dipolar coupling between 1329Si and 13C nuclei exists.