Correlative light and scanning electron microscopy of the same sections gives new insights into the effects of pectin lyase on bordered pit membranes in Pinus radiata wood

Bordered pits are structures in the cell walls of softwood tracheids which permit the movement of water between adjacent cells. These structures contain a central pit membrane composed of an outer porous ring (margo) and an inner dense and pectin-rich disc (torus). The membrane is overarched on each side by pit borders. Pits may be aspirated, a condition where the torus seals against the pit border, effectively blocking the pathway between cells. In living trees this maintains overall continuity of water conduction in xylem by sealing off tracheids containing air. Drying of timber results in further pit aspiration, which reduces wood permeability to liquid treatment agents such as antifungal chemicals. One possible way to increase permeability is by treating wood with pectin lyase to modify or remove the torus. The effectiveness of this treatment was initially evaluated using light microscopy (LM) of toluidine blue stained wood. Pectic material is coloured pink-magenta with this stain, and loss of this colour after treatment has been interpreted as indicating destruction of the torus. However, correlative light (LM) and scanning electron (SEM) microscopic observations of identical areas of toluidine blue stained sections revealed that many unstained pits had intact but modified tori when viewed with SEM. These observations indicate that LM alone is not sufficient to evaluate the effects of pectin lyase on pit membranes in wood. Combining LM and SEM gives more complete information.     

Copper-carbon nanocomposites prepared by sold-phase pyrolysis of copper phthalocyanine

By using solid-phase pyrolysis of copper phthalocyanine we have prepared copper nanoparticles in carbon matrices. The elemental composition, structure, and morphology of nanocomposites were investigated by scanning electron microscopy, energy dispersive X-ray microanalysis, and X-ray diffraction. Depending on the temperature and time of pyrolysis, the sizes of copper nanoparticles can be varied from 10 nm to 400 nm. The structure of carbon matrices also strongly depends on the pyrolysis conditions, which allows us to synthesize nanocomposites with given properties.     

Investigation of carbon microspheres prepared by solid-phase pyrolysis of metal-free phthalocyanine

By using solid-phase pyrolysis of metal-free phthalocyanine (H₂C₃₂N₈H₁₆) we have prepared carbon microspheres with a mean diameter from 2–3.5 μm and sufficiently narrow size distribution. The elemental composition, structure and morphology of samples were studied by scanning electron microscopy, energy-dispersive X-ray microanalysis, and X-ray diffraction. A strong electron paramagnetism was revealed in microspheres.     

Preparation and characterization of nickel nanoparticles in different carbon matrices

Using the solid-phase pyrolysis and chemical vapor deposition of nickel-phthalocyanine, we have fabricated ferromagnetic Ni nanoparticles in carbon matrices. The composition, structure, morphology, and magnetic properties of samples were investigated by means of scanning electron microscopy, energy dispersive X-ray microanalysis, X-ray diffraction technique, and ferromagnetic resonance. It is shown that the sizes of nanoparticles can be varied from ∼10 nm to ∼500 nm depending on the temperature and time of pyrolysis. The used method allows us to synthesize metal nanoparticles in different carbon matrices: in amorphous carbon plates, in graphitic capsules, and in carbon nanotubes.     

Wood surface functionalization by means of low-pressure air plasma

Low-pressure plasma treatments in an radio frequency (RF) discharge of air have been used on the surface of wood to stimulate polar function groups onto pine and beach surfaces to enhance the wettability and activation. The effects of plasma treatments on the morphology and wettability of surfaces were characterized by using static contact angle measurements, attenuated total reflection Fourier transform infrared spectroscopy and scanning electron microscopy. A clear increase in the surface energy of the wood surface due to air plasma treatment was observed. The surfaces became highly hydrophilic when woods were exposed for 5 s or longer to the plasma discharge. The wettability of wood surface can be improved when oxygen functionalities were generated, which can be achieved directly in O-containing plasma or via post plasma reaction. A small reduction in the surface energy of the treated wood after 12 days of aging showed that the plasma-induced cross-linking in the surface of the wood was not the dominant phenomenon.     

Forced Air Plasma Treatment (FAPT) of Hybrid Wood Plastic Composite (WPC)–Fiber Reinforced Plastic (FRP) Surfaces

Forced atmospheric (air) plasma treatment (FAPT) was applied to wood plastic composite (WPC) and continuous glass fiber reinforced plastic (FRP) surfaces to improve their adhesive bonding properties. The FRP was composed of oriented continuous E-glass fibers in a polypropylene matrix, while the WPC was fabricated using wood flour, polypropylene and additives. The FAPT was applied using two levels of discharge length projected from the discharge head (2.5″ and 1″) to ionize the air, oxidize the surfaces and improve wettability. The treatment was performed by passing the electrode over either surface, five or ten times. Surface characterization consisted of thermodynamic (surface energy determination), chemical (X-ray photoelectron spectroscopy), mechanical (shear strength) and microscopic (atomic force microscopy (AFM)) analysis. The results indicate that the acid–base component of the surface energy for both WPC and FRP after FAPT correlates with an increase in wettability. X-ray photoelectron spectroscopy was performed on wood regions and non-wood regions of the WPC surfaces; the oxygen concentration increased to a larger extent in the non-wood regions. Bonding shear strength measurements indicated increases of 50% after FAPT on WPC surfaces (2.5″ discharge length, 1 pass) and up to 200% for the hybrid WPC–FRP. Atomic force microscopy measurements using a silicon tip probe showed increases in adhesive force interactions up to 56% on WPC surfaces post-FAPT.     

Surface composition of the steel powders pre-alloyed with manganese

The determination of the surface oxide layer composition is vital to facilitate the adjustment of the sintering conditions for sufficient removal of the surface oxides for providing strong metal bonding between the metal particles during sintering. To systematically investigate the composition, morphology and thickness of the surface oxide the influence of manganese content from 0.3 to 1.8 wt.% on the surface products composition in the case of water atomized steel powder was evaluated. Analysis of the powder surfaces by X-ray photoelectron spectroscopy and high-resolution scanning electron microscopy in combination with X-ray microanalysis showed that powder particles in all cases are covered by heterogeneous oxide layer, composed of particulate features of thermodynamically stable oxides (Cr-Mn-Si) and homogeneous iron surface oxide layer in between. For increasing alloying content the fraction of stable oxide cations in the surface layer increases linearly, whereas the thickness of the iron oxide layer decreases. Moreover, from the investigation of the sintering and degassing behavior by thermal analysis coupled with mass-spectrometry (TG/DTA + MS), three different stages of carbothermal reduction process were observed and their correlation with surface oxides composition was established during sintering in argon.     

Sonochemical synthesis of iron phosphide

The sonochemical reaction of Fe(CO)5 and triethylphosphine has been found to produce solid amorphous iron phosphide of composition FeP. The resulting compound was characterized by elemental microanalysis, scanning electron microscopy, energy-dispersive X-ray analysis, and Debye-Scherrer powder X-ray diffraction. X-ray powder patterns were obtained after the amorphous material had been heated above 950 degrees C and then slowly cooled to induce crystallization. This reaction provides the first use of ultrasound to sonochemically synthesize amorphous phosphide semiconductor materials from organometallic precursors.     

Investigation of Ceramic-Like Coatings Formed on Aluminum Composites by Microarc Oxidation

Ceramic-like coatings with a thickness of up to 40 μm are formed on aluminum composites without additives and with copper additives (1 and 4.5%) in a silicate-alkaline electrolyte by microarc oxidation. The composites are prepared by powder metallurgy (cold pressing and sintering in forevacuum). An increase in the copper concentration in the composites to 4.5% leads to the retardation of anode voltage growth on the initial stage of oxidation corresponding to the formation of a barrier layer. The coatings are studied by scanning electron microscopy, X-ray microanalysis, X-ray photoelectron spectroscopy, and X-ray diffraction. The morphology of their surface corresponds to the morphology of the surface of coatings on compact aluminum alloys. According to X-ray photoelectron spectroscopy, a thin 1-μm layer forms on the surface. It consists predominantly of electrolyte components. X-ray diffraction analysis shows that the coatings mainly consist of γ-Al₂O₃ oxide as well as the η-Al₂O₃ phase, the peaks of which are broadened. This broadening is characteristic of the amorphous component and may be due to the presence of nanocrystalline regions in the coating structure. In the coatings on the composite Al + 4.5% Cu, mullite Al₂SiO₅ and copper oxide CuO are also found. The excess aluminum content may be associated with residual unoxidized aluminum inclusions in the structure of the coatings.     

Wood typification by Venturi easy ambient sonic spray ionization mass spectrometry: the case of the endangered Mahogany tree

Venturi easy ambient sonic spray ionization mass spectrometry in both its liquid (V(L) -EASI-MS) and solid sample modes (V(S) -EASI-MS) is shown to provide nearly immediate and secure typification of woods, as demonstrated for Mahogany, an endangered and most valuable type of tropical wood. This reddish wood displays unique phytochemical markers (phragmalin-type limonoids) which are rapidly detected from the wood surface by V(S) -EASI-MS or from a simple methanol extract of a tiny wood chip by V(L) -EASI-MS. Unique profiles were obtained for Mahogany (Swietenia macrophylla) whereas genuine samples of six other similar types of woods, which are commonly falsified by artificial coloring and commercialized as Mahogany, display also typical but dissimilar pythochemical profiles as compared to that of the authentic wood. Variable and atypical chemical profiles were observed for artificially colored woods. Secure chemical characterization via V(S) -EASI-MS or V(s) -EASI-MS fingerprints of Mahogany and other types of woods with similar appearance should help to control the illegal logging and trade of this and other endangered woods and their falsification, and to create certified standards.     

Investigation of the composition and properties of catalytic layers prepared by the ion beam-assisted deposition of tin and platinum on carbon supports

Catalytic layers are prepared by the vacuum ion-beam-assisted deposition of tin and platinum onto carbon-based AVCarb® Carbon Fiber Paper P50 and Toray Carbon Fiber Paper TGP-H-060 T supports to produce electrocatalysts for direct methanol and ethanol fuel cells with a polymer-membrane electrolyte. The layers are formed in the mode of ion-assisted deposition, wherein ions of the deposited metal are used as ions assisting deposition. Metal deposition is performed from a neutral vapor fraction, while mixing of the deposited layer with the substrate by accelerated ions of the same metal is carried out from the vacuum arc discharge plasma of a pulsed electric arc ion source. The morphology and composition of the layers is studied using scanning electron microscopy, electron probe microanalysis, X-ray fluorescence analysis, and Rutherford backscattering spectrometry. It is demonstrated by means of voltammetric measurements that the resulting electrocatalysts exhibit activity in the oxidation of methanol and ethanol.     

Supercritical Fluid Extraction as a Method of Thermochemical Activation of Wood Cell Walls

The thermochemical activation of the lignocarbohydrate matrix by supercritical (SC) fluid extraction was studied. Labile and stable regions of lignocarbohydrate formations distributed in the cell wall were revealed. Changes in the composition and morphology of the wood substance during the treatment were determined. Supercritical fluid extraction with carbon dioxide was shown to be a useful method for selective treatment of the weak H-bonds of the lignocarbohydrate complex to obtain new data on the structure and composition of the wood substance and its components.     

Electron microscopic studies of single crystal inclusions in pyroboroncarbon

A study of the composition and structure of large single crystal inclusions formed inside cavities in pyroboroncarbon by means of energy dispersive X-ray microanalysis and electron diffraction analysis shows that they correspond to one phase of rhombohedral boron carbide. Bright-field images obtained by transmission electron microscopy show that their growth continues throughout the technological cycle of material growth due to the diffusion of boron atoms from the pyrocarbon phase of pyroboroncarbon adjacent to the cavities.     

LC-DAD/ESI-MS/MS study of phenolic compounds in ash (Fraxinus excelsior L. and F. americana L.) heartwood. Effect of toasting intensity at cooperage

The phenolic composition of heartwood extracts from Fraxinus excelsior L. and F. americana L., both before and after toasting in cooperage, was studied using LC-DAD/ESI-MS/MS. Low-molecular weight (LMW) phenolic compounds, secoiridoids, phenylethanoid glycosides, dilignols and oligolignols compounds were detected, and 48 were identified, or tentatively characterized, on the basis of their retention time, UV/Vis and MS spectra, and MS fragmentation patterns. Some LMW phenolic compounds like protocatechuic acid and aldehyde, hydroxytyrosol and tyrosol, were unlike to those for oak wood, while ellagic and gallic acid were not found. The toasting of wood resulted in a progressive increase in lignin degradation products with regard to toasting intensity. The levels of some of these compounds in medium-toasted ash woods were much higher than those normally detected in toasted oak, highlighting vanillin levels, thus a more pronounced vanilla character can be expected when using toasted ash wood in the aging wines. Moreover, in seasoned wood, we found a great variety of phenolic compounds which had not been found in oak wood, especially oleuropein, ligstroside and olivil, along with verbascoside and isoverbascoside in F. excelsior, and oleoside in F. americana. Toasting mainly provoked their degradation, thus in medium-toasted wood, only four of them were detected. This resulted in a minor differentiation between toasted ash and oak woods. The absence of tannins in ash wood, which are very important in oak wood, is another peculiar characteristic that should be taken into account when considering its use in cooperage.     

The effect of ultrasonic intensity on physicochemical properties of Chinese fir

Cavitation intensity is affected by ultrasonic intensity (UI) and is a key parameter to describe experimental results during ultrasonic treatment. The relationship between the UI and physicochemical properties of Chinese fir was investigated. In this study, four frequencies (25, 28, 40, and 59 kHz) were used at the same intensity of 240 W and the same duration of 35 min. The UI during the ultrasonic treatment was determined, and the chemical components were determined. The chemical structure, crystallinity, morphology, and extractives of wood were respectively analyzed by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and gas chromatography-mass spectrometry (GC–MS). The results showed that higher crystallinity was associated with a larger integrated area under the curve of the ultrasonic intensity (UIA). The largest UIA was observed at 25 kHz, followed by those at 40, 59, and 28 kHz. The relative content of hemicellulose was strongly affected by the ultrasonic treatment. No chemical reactions were observed in the wood, whereas the ultrasonic treatment affected the torus of the bordered pits and facilitated the migration of extractives. In general, the higher the UIA, the stronger the effect of the cavitation was. The most significant changes in the physicochemical properties were observed at 25 kHz. The instantaneous ultrasonic intensity (IUI) changed over time, and the UIA was closely associated with changes in the physicochemical properties of the wood. The results of this study demonstrate that UI has a significant influence on the physicochemical properties of wood.     

Structural and spectroscopic analysis of hot filament decomposed ethylene deposited at low temperature on silicon surface

The deposition of decomposed ethylene on silicon wafer at lower temperature using hot filament chemical vapor deposition (HFCVD) method was applied to compose thin film of carbon and its compounds with silicon and hydrocarbon structures. The films were analyzed using Raman spectroscopy, X-ray diffraction, and scanning electron microscopy with elemental microanalysis by energy dispersive X-ray spectrometer. The structure and morphology of the early stage of the film deposition was analyzed. The obtaining of SiC as well as diamond-like structure with this method and catalytic influence of chemical admixtures on the film structure and properties are discussed.     

Acoustical classification of woods for string instruments

Two basic types of wood are used to make stringed musical instruments: woods for soundboards (top plates) and those for frame boards (back and side plates). A new way to classify the acoustical properties of woods and clearly separate these two groups is proposed in this paper. The transmission parameter (product of propagation speed and Q value of the longitudinal wave along the wood grain) and the antivibration parameter (wood density divided by the propagation speed along the wood grain) are introduced in the proposed classification scheme. Two regression lines, drawn for traditional woods, show the distinctly different functions required by soundboards and frame boards. These regression lines can serve as a reference to select the best substitute woods when traditional woods are not available. Moreover, some peculiarities of Japanese string instruments, which are made clear by comparing woods used for them with woods used for Western and Chinese instruments, are briefly discussed.     

Fabrication of superhydrophobic wood surfaces via a solution-immersion process

Superhydrophobic wood surfaces were fabricated from potassium methyl siliconate (PMS) through a convenient solution-immersion method. The reaction involves a hydrogen bond assembly and a polycondensation process. The silanol was formed by reacting PMS aqueous solution with CO₂, which was assembled on the wood surface via hydrogen bonds with the wood surface -OH groups. The polymethylsilsesquioxane coating was obtained through the polycondensation reaction of the hydroxyl between wood and silanol. The morphology of products were characterized using a scanning electron microscope (SEM), the surface chemical composition was determined using energy dispersive X-ray analysis (EDXA), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry (TGA) and contact angle measurement. Analytical results revealed that rough protuberances uniformly covered the wood surface, thus transforming the wood surface from hydrophilic to superhydrophobic. The water contact angle of the superhydrophobic wood surface was about 153° and a sliding angle was 4.6°.     

X-Ray fluorescence analysis using synchrotron radiation of manganese minerals from marine and lake bottom sediments

We perform X-ray fluorescence analysis of ferromanganese crusts from regions of the Okhotsk and Bering Seas and the Lake Miassovo (Southern Urals) with different geological structures using synchrotron radiation combined with X-ray diffraction and infrared spectroscopy (SR XRF). The consistency of the minor element composition to the structural patterns of manganese minerals of investigated samples is demonstrated.