WOOD SCIENCE AND TECHNOLOGY

Conservation of model degraded pine wood with selected organosilicons studied by XFM and nanoindentation
Broda M, Jakes JE, Li L, Antipova OA, Maxey ER and Jin Q
Studies on new conservation agents for waterlogged archeological wood require vast amounts of similar wooden material. Therefore, model wood is useful for this purpose. The goal of the present research was to determine the mechanism of wood stabilization by organosilicon compounds to understand their mode of action and thus inform how to more effectively apply them to preserve various wooden artifacts. The study used chemically (ChP) and biologically degraded (BP) model Scots pine wood treated with Methyltrimethoxysilane (MTMS), (3-Mercaptopropyl)trimethoxysilane (MPTMS), or 1,3-Bis(diethylamino)-3-propoxypropanol)-1,1,3,3-tetramethyldisiloxane (DEAPTMDS). Synchrotron-based X-ray fluorescence microscopy (XFM) was used to investigate the penetration of organosilicons into the wood cellular structure and cell walls, and nanoindentation was used to study the mechanical properties of the treated wood cell walls. All treatments resulted in high volumetric anti-shrink efficiency (ASE) values of 74-82%, except for MTMS-treated ChP with an ASE of 52%. The multiscale XFM results revealed that all applied organosilicons penetrated throughout the whole wooden blocks and deposited in both cell lumina and cell walls. The retention of all applied organosilicons was highest in BP wood, and so was the dimensional stabilization effect. MTMS-treated ChP had the lowest measured cell wall infiltration, which likely contributed to its lower ASEv. DEAPTMDS treatments plasticized the cell walls and resulted in lowered nanoindentation elastic modulus ( ) and hardness () for all types of wood. MTMS and MPTMS had modest effects on cell wall mechanical properties and the effect depended on the type or wood. The final effect of organosilicon treatment on the dimensional wood stabilization and mechanical properties of wood cell walls depended not only on the type of the applied organosilicon, but also the properties of treated wood. This means that the treatment cannot be considered universal and individual approach is needed for the conservation of individual wooden objects. Although some mechanisms are now better understood, such as the need for organosilicons to infiltrate the cell walls and the plasticizing effect of DEAPTMDS, other aspects will benefit from more detailed analysis of the molecular interactions between organosilicons and wood polymers.
Impregnation of Scots pine and beech with tannin solutions: effect of viscosity and wood anatomy in wood infiltration
Tondi G, Thevenon MF, Mies B, Standfest G, Petutschnigg A and Wieland S
The impregnation process of Scots pine and beech samples with tannin solutions was investigated. The two materials involved in the process (impregnation solution and wood samples) are studied in depth. Viscosity of mimosa tannin solutions and the anatomical aspect of beech and Scots pine were analysed and correlated. The viscosity of tannin solutions presents a non-newtonian behaviour when its pH level increases, and in the case of addition of hexamine as a hardener, the crosslinking of the flavonoids turns out to be of great importance. During the impregnation of Scots pine ( L.) and beech ( L.), the liquid and solid uptakes were monitored while taking into consideration the different conditions of the impregnation process. This method allowed to identify the best conditions needed in order to get a successful preservative uptake for each wooden substrate. The penetration mechanism within the wood of both species was revealed with the aid of a microscopic analysis. Scots pine is impregnated through the tracheids in the longitudinal direction and through parenchyma rays in the radial direction, whereas in beech, the penetration occurs almost completely through longitudinal vessels.
Fracture behaviour of historic and new oak wood
Luimes RA, Suiker ASJ, Verhoosel CV, Jorissen AJM and Schellen HL
Recent museum studies have indicated the appearance of cracks and dimensional changes on decorated oak panels in historical Dutch cabinets and panel paintings. A thorough analysis of these damage mechanisms is needed to obtain a comprehensive understanding of the causes of damage and to advise museums on future sustainable preservation strategies and rational guidelines for indoor climate specifications. For this purpose, a combined experimental-numerical characterization of the fracture behaviour of oak wood of various ages is presented in this communication. Three-point bending tests were performed on historical samples dated 1300 and 1668 A.D. and on new samples. The measured failure responses and fracture paths are compared against numerical results computed with a finite element model. The discrete fracture behaviour is accurately simulated by using a robust interface damage model in combination with a dissipation-based path-following technique. The results indicate that the samples dated 1300 A.D. show a quasi-brittle fracture response, while the samples dated 1668 A.D. and the new samples show a rather brittle failure response. Further, the local tensile strength of the oak wood decreases with age in an approximately linear fashion, thus indicating a so-called ageing effect. Numerical simulations show that, due to small imperfections at the notch tip of the specimen, the maximal load carrying capacity under three-point bending may decrease by maximally . A comparison between a calibration of the experimental results by isotropic and orthotropic elastic models shows that the peak load is 10- higher for the orthotropic elastic model. Finally, no significant dependence of the fracture toughness on the age of the oak wood and on the orientation of the fracture plane has been found. The strength and toughness values measured can be used as input for advanced numerical simulations on climate-induced damage in decorated oak wooden panels and panel paintings.
Differentiation between pine woods according to species and growing location using FTIR-ATR
Traoré M, Kaal J and Martínez Cortizas A
Attenuated total reflectance-Fourier transform infrared (FTIR-ATR) spectroscopy was applied to 120 samples of heartwood rings from eight individual pine trees from different locations in Spain. cores were collected at the Artikutza natural park (Ps-ART). cores were collected in Sierra de Cazorla (Pn-LIN) and in La Sagra Mountain (Pn-LSA). Three discriminant analysis tests were performed using all bands (DF), lignin bands only (DF) and polysaccharides bands only (DF), to explore the ability of FTIR-ATR to separate between species and growing location. The DF model enabled a good separation between pine species, whereas the DF model enabled differentiation for both species and growing location. The DF model enabled virtually perfect separation, based on two functions involving twelve FTIR bands. Discrimination between species was related to bands at 860 and 1655 cm, which were more intense in samples, and bands at 1425 and 1635 cm, more intense in samples. These vibrations were related to differences in lignin structure and polysaccharide linear chains. Discrimination between growing locations was mainly related to polysaccharide absorptions: at 900, 1085 and 1335 cm more representative of Pn-LIN samples, and at 1105 and 1315 cm mostly associated to Pn-LSA samples. These absorptions are related to β-glycosidic linkages (900 cm), cellulose and hemicellulose (C-O bonds, 1085 and 1105 cm) and content in amorphous/crystalline cellulose (1315 and 1335 cm). These results show that FTIR-ATR in combination with multivariate statistics can be a useful tool for species identification and provenancing for pine wood samples of unknown origin.
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Enhanced water uptake in the longitudinal direction by shiitake mycelium in shiitake cultivation logs: increase in effective diffusion coefficient based on mass of liquid water uptake
Ogawa K and Yashima T
In the cultivation of shiitake mushrooms (), the farmer needs to know the time needed to water in order to adjust the water content of the logs. In this study, six test logs (, diameter of 38-48 mm, length of 110-118 mm) were used, of which some were dried, some had shiitake mycelia grown on them, and some had mold generated on them. Liquid water was supplied to the test logs by placing the longitudinal direction of the test logs along the line of gravity and immersing the bottom of the test logs in water. Water uptake mass of the test logs was measured for 20 h. The effective diffusion coefficient, , was calculated from the change in time of the water uptake mass using Fick's diffusion law. The of test logs in which shiitake mycelium grew were 1.5-3.4 × 10 m/s, and the values were 2.4-4.7 times higher than that for the dried log. On the other hand, the of the moldy logs were 6.7-9.7 × 10 m/s, which was 0.058-0.081 times that of dry test logs. Based on observation of water penetration into logs by magnetic resonance imaging (MRI) and an optical microscope, it is believed that the driving force behind liquid water rising in the longitudinal direction in the test log is the capillary force acting on a three-phase interface consisting of the inner wall surface of the vessel, liquid water and air.
Sulfation of arabinogalactan with sulfamic acid under homogeneous conditions in dimethylsulfoxide medium
Levdansky AV, Vasilyeva NY, Kondrasenko AA, Levdansky VA, Malyar YN, Kazachenko AS and Kuznetsov BN
Sulfation of larch wood arabinogalactan (AG) with sulfamic acid in dimethylsulfoxide (DMSO) medium in the presence of urea was studied for the first time. The use of DMSO as a solvent instead of more toxic 1,4-dioxane allows to sulfate AG under homogeneous conditions. The sulfated AG with a high sulfur content (12.0-12.5 wt %) was produced by sulfation at a temperature of 85-90 °C, the molar ratio of AG / sulfating agent equal to 1:0.85 during 2-3 h. The introduction of sulfate groups into the structure of arabinogalactan was confirmed by the appearance of new absorption bands in FTIR and FT Raman spectra, characteristic for the vibrations of the sulfate groups. It was proved by C NMR spectroscopy that the predominant substitution of the primary hydroxyl groups at C6 carbon atoms of the terminal galactose units of main and side chains of arabinogalactan takes place. Simultaneously, the hydroxyl groups associated with C2 and C4 carbon atoms of galactose unit of the main chain are only partially sulfated. According to results of GPC study, the sulfated AG is characterized by a narrow molecular weight distribution with an average molecular weight of 18.8 kDa and a polydispersity of 1.3.
Enhanced water uptake in the longitudinal direction by shiitake mycelium in shiitake cultivation logs: water content distribution in logs measured by magnetic resonance imaging
Ogawa K and Yashima T
In the cultivation of shiitake mushrooms (), the farmer needs to know the time needed to water in order to adjust the water content of the logs. To study the enhanced water uptake in the longitudinal direction by shiitake mycelium in shiitake cultivation logs, six dried test logs (, diameter of 38 to 48 mm, length of 110 to 118 mm) were used. Three test logs had shiitake mycelium grown on them, and the remaining three test logs had mold generated on them. Liquid water was supplied to the bottom surface of the test log which had its longitudinal direction along the line of gravity. Water content distribution in the logs was measured in chronological order using magnetic resonance imaging (MRI) with 1 Tesla. The calibration curve for converting the signal intensity of the MR image into the water content in the test log was determined by cutting the test log at 5-mm intervals and measuring the water content distribution using the mass method. Spatial distribution of the water content of the test log without shiitake mycelium depending on the cumulative water supply time was obtained, and the distribution shape was always concave corresponding to the exact solution of an unsteady one-dimensional diffusion equation with one diffusion coefficient. In the case of the test log in which shiitake mycelium grew, within a few hours after liquid water supply the water content increased in the whole region where shiitake mycelium grew, and the shape of the water content distribution in the longitudinal direction became convex. Based on observation of water penetration into logs by MRI and an optical microscope, it is believed that the driving force behind increased rise in liquid water in the longitudinal direction in the test log is the capillary force acting in vessels.
Prediction of moisture-induced cracks in wooden cross sections using finite element simulations
Brandstätter F, Autengruber M, Lukacevic M and Füssl J
Wood absorbs and desorbs moisture due to its hygroscopic behavior, leading to moisture gradients in timber elements as well as swelling and shrinkage. These processes are constrained due to the orthotropic material properties of wood, leading to moisture-induced stresses, which can cause crack initiation and propagation. A significant amount of the damage in timber constructions indoors can be related to changes of the moisture content (MC). However, more information is needed about the correlation between moisture changes or gradients and specific damage characteristics, like crack depths. Thus, based on numerical simulations, the crack depth development within two solid timber and one glued laminated timber (GLT) cross section over time for different relative humidity (RH) reductions and initial MCs is analyzed. For this purpose, a multi-Fickian transport model is used to determine moisture fields, which are then used as loads in a subsequent stress simulation, where linear elastic material behavior is considered. An extended finite element approach, supported by a multisurface failure criterion defining the failure behavior, allows for the simulation of moisture-induced discrete cracking. Based on simulation results, correlations between potential maximum crack depths and moisture gradients in indoor climate conditions are derived, which enables the prediction of crack depths in wood. Finally, it is shown that the initial MC level significantly influences the maximum crack depth that can be expected.
Green and sustainable fabrication of DES-pretreated high-strength densified wood
Gondaliya AM, Hoque M, Raghunath S and Foster EJ
Wood is a sustainable, benign, and high-performing green structural material readily available in nature that can be used to replace structural materials. However, insufficient mechanical performance (compared to metals and plastic), moisture sensitivity, and susceptibility to microorganism attack make it challenging to use wood as it is for advanced engineering applications. We here present an efficient approach to fabricating densified wood with minimal time and waste generation, demonstrating high mechanical strength, and decreased water penetration on the surface. Wood slabs were treated with deep eutectic solvents (DESs) to solubilize the lignin, followed by in-situ regeneration of dissolved lignin in the wood. Then, the slabs were densified with heat and pressure, turning the wood into a functionalized densified material. Lignin regeneration and morphological changes were observed via two-photon microscopy and Scanning Electron Microscopy (SEM), respectively. The final product is less susceptible to water absorption on the surface and has enhanced flexural strength (> 50% higher), surface hardness (100% increased), and minimal set recovery compared to natural wood. The improved mechanical performance is due to regenerated lignin which acts as a glue and fills spaces present within the interconnected cellulose network inside the wood, forming a highly dense composite during densification. Such enhancement in the properties of DES-densified wood composite makes it a favorable candidate for advanced structural and engineering applications.
Investigation of cyclic water infiltration and dry-out in coated spruce using finite-element simulations
Brandstätter F, Senoner M, Lukacevic M, Autengruber M, Truskaller M, Grüll G and Füssl J
Accurate prediction of moisture distributions in wood is among the most critical challenges in timber engineering. Achieving this requires a well-coordinated comparison of experimental methods and simulation tools. While significant progress has been made in developing simulation tools in recent years, a lack of experience with and trust in these tools continues to hinder broader implementation, especially when it comes to free water and its absorption. Investigations and model advancements have allowed for the simulation of increasingly complex cases, including one-dimensional moisture transport above the fiber saturation point (FSP) in coated boards and below FSP in coated glued laminated timber (GLT). However, free water flow in coated GLT beams has not yet been addressed, which can become problematic in case of extreme scenarios, such as water infiltration. In this study, we demonstrate that the multi-Fickian free water transport model developed by some of the authors can successfully simulate three-dimensional coated cases. Uncoated and coated boards and GLT members were subjected to cyclic wetting and drying, both experimentally and numerically. To simplify the calibration process of the mass transfer coefficient of free water-identified as the most significant parameter for the simulation of free water transport-experiments previously conducted by some of the authors were simulated. Based on the simulation results, approaches for an initial estimation of the mass transfer coefficient were developed. If the water uptake of coated specimens is measured three days after continuous soaking in water and the result exceeds a specific limit, the coefficient can be sufficiently predicted. The simulation and experimental results show a good agreement.
Level set-based image segmentation of CT scanned oak micro-structures with an analysis of morphological features
Livani MA, Suiker ASJ and Bosco E
A three-dimensional level set-based image segmentation method is presented for a robust identification and accurate characterization of the different cell types defining complex wood micro-structures. The method can be applied to arbitrary wood species, and in this contribution is elaborated for oak. The evolution of the level set function and the corresponding boundary conditions are rigorously derived from a variational framework based on the Local Chan-Vese energy functional. The application of the level-set image segmentation approach enables to distinguish the cell wall material from the cell cavities. The cell material objects are subsequently segmented into axial cell objects and ray parenchyma cell objects that are oriented in the longitudinal and radial material directions of oak wood, respectively. This additional segmentation step facilitates the collection of statistical information on the inner cell dimensions and wall thickness of axial cells and ray parenchyma cells from images taken across principal material planes of the oak micro-structure. The performance and results of the image segmentation method are analyzed by using as input detailed micro-structural images of two representative oak samples containing a single growth ring, as obtained from X-ray micro-computed tomography experiments. The assessment of the robustness and convergence behaviour of the image segmentation method shows that the method converges very fast into a unique oak micro-structure that is independent of the initial configuration selected. The accuracy of the image segmentation result is shown through a comparison with the results obtained by two other image segmentation methods presented in the literature, and by visualizing and identifying small-scale morphological features within oak growth rings in great detail. The computational cost of the image segmentation method is evaluated by comparing its performance on CPU and GPU hardware. Additionally, a statistical analysis is carried out of the maximum and minimum inner cell diameters and the cell wall thickness of the various axial cells-fibers and axial parenchyma, earlywood vessels, latewood vessels-and ray parenchyma cells defining the micro-structure of the oak growth ring samples. The density histograms constructed for these geometrical parameters provide their statistical spread and most frequent value, which are quite similar for the two oak samples and are in good agreement with other experimental data reported in the literature. The oak micro-structures identified and characterized by the present image segmentation method may serve as input for dedicated finite element models that compute their mechanical/physical behaviour as a function of the geometrical and physical properties of the individual cells.