Backscattered Electron Mode Research Articles

Electron microscopy of the primary microstructure of rapidly solidified Ti-46Al-8Nb alloy

The contradictory data on the formation of the microstructure of a refractory intermetallic Ti-46 at % Al-8 at % Nb alloy and on the phase transformations proceeding within in the Ti-Al-Nb phase diagram are analyzed and improved experimentally. To determine the primary solidified phase, a set of experiments is performed on melting of the alloy, which is synthesized in a high-purity argon atmosphere using crucibles made of an oxygen-free ceramics (99.99% AlN), and subsequent rapid volumetric isothermal solidification. Cooling from 1943 K at rates of 5, 10, and 20 K/s and subsequent quenching from 1763 K are used. Polished sections of ingots are studied by scanning electron microscopy using backscattered electron mode. Scanning electron microscopy micrographs demonstrate contrast regions of nonuniform niobium segregation, which are fixed by quenching and decorate the primary polycrystalline microstructure formed in the temperature range from 1843 (liquidus) to 1773 K (solidus). The primary crystalline phase is shown to be represented by β(Ti) dendrites, which have clearly pronounced fourfold symmetry that form during the development of secondary arms.

Annealing behavior of ferritic–martensitic 9%Cr–ODS–Eurofer steel

Oxide dispersion strengthened ferritic–martensitic steels are potential candidates for applications in future fusion power plants. High creep resistance, good oxidation resistance, reduced neutron activation and microstructural long-term stability at temperatures of about 650–700 °C are required in this context. In order to evaluate its thermal stability in the ferritic phase field, samples of the reduced activation ferritic–martensitic 9%Cr–ODS–Eurofer steel were cold rolled to 50% and 80% reductions and further annealed in vacuum from 300 to 800 °C for 1 h. The characterization in the annealed state was performed by scanning electron microscopy in the backscattered electron mode, high-resolution electron backscatter diffraction and transmission electron microscopy. Results show that the fine dispersion of Y-based particles (about 10 nm in size) is effective to prevent recrystallization. The low recrystallized volume fraction (<0.1) is associated to the nuclei found at prior grain boundaries and around large M 23C 6 particles. Static recovery was found to be the predominant softening mechanism of this steel in the investigated temperature range.

First detection of lead in black paper from intraoral film: An environmental concern

Lead (Pb) contamination in the black paper that recovers intraoral films (BKP) has been investigated. BKP samples were collected from the Radiology Clinics of the Dental School of Ribeirão Preto, University of São Paulo, Brazil. For sake of comparison, four different methods were used. The results revealed the presence of high lead levels, well above the maximum limit allowed by the legislation. Pb contamination levels achieved after the following treatments: paper digestion in nitric acid, microwave treatment, DIN38414-54 method and TCLP method were 997 μg g −1, 189 μg g −1, 20.8 μg g −1, and 54.0 μg g −1, respectively. Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma mass spectrometry (ICP-MS) were employed for lead determination according to the protocols of the applied methods. Lead contamination in used BKP was confirmed by scanning electron microscopy coupled with energy dispersive X-ray microanalysis (SEM-EDS). All the SEM imaging was carried out in the secondary electron mode (SE) and backscattered-electron mode (QBSD) following punctual X-ray fluorescence spectra. Soil contamination derived from this product revealed the urgent need of addressing this problem. These elevated Pb levels, show that a preliminary treatment of BKP is mandatory before it is disposed into the common trash. The high lead content of this material makes its direct dumping into the environment unwise.

Effect of 2% chlorhexidine on dentin microtensile bond strengths and nanoleakage of luting cements

Objectives The aim of this study was to investigate the effect of pre-treatment by chlorhexidine on the microtensile bond strength (mTBS) of resin cements and nanoleakage at the resin–dentine interfaces. Methods Cylindrical composite blocks were luted to human dentine using resin cements (RelyX ARC, 3M ESPE: ARC; Panavia F, Kuraray Medical Inc.: PF; RelyX Unicem, 3M ESPE: UN) with/without pre-treatment by 2% chlorhexidine digluconate (CAVITY CLEANSER, Bisco, Inc., Schaumburg, IL, USA). CAVITY CLEANSER was applied on the acid etched dentine for 60 s in the ARC group, and on smear layer-covered dentine in the PF and UN groups. After storage in water for 24 h, the bonded teeth were sectioned into 1 mm thick slabs and further into 0.9 mm × 0.9 mm beams. After immersion in water or ammoniacal silver nitrate for 24 h, the beams were stressed to failure in tension. The fractured surfaces were examined by field-emission scanning electron microscopy (FE-SEM) using backscattered electron mode. The silver-stained slabs were used to examine nanoleakage within the bonded interface by FE-SEM. Results The resin cement and chlorhexidine treatment had significant effects ( p < 0.0001) on mTBS; while the storage media had no significant effect ( p = 0.435). The mTBS of ARC was significantly higher than the other cements. Chlorhexidine reduced mTBS and produced pronounced nanoleakage when PF and UC were luted to dentine. Conclusions Pre-treatment with chlorhexidine affected the integrity of dentine bonding with PF and UC, while there was no adverse effect on coupling of ARC.

Double fossilization in eukaryotic microorganisms from Lower Cretaceous amber

BackgroundMicrofossils are not only useful for elucidating biological macro- and microevolution but also the biogeochemical history of our planet. Pyritization is the most important and extensive mode of preservation of animals and especially of plants. Entrapping in amber, a fossilized resin, is considered an alternative mode of biological preservation. For the first time, the internal organization of 114-million-year-old microfossils entrapped in Lower Cretaceous amber is described and analyzed, using adapted scanning electron microscopy in backscattered electron mode in association with energy dispersive X-ray spectroscopy microanalysis. Double fossilization of several protists included in diverse taxonomical groups and some vegetal debris is described and analyzed.ResultsIn protists without an exoskeleton or shell (ciliates, naked amoebae, flagellates), determinate structures, including the nuclei, surface envelopes (cortex or cytoplasmic membrane) and hyaloplasm are the main sites of pyritization. In protists with a biomineralized skeleton (diatoms), silicon was replaced by pyrite. Permineralization was the main mode of pyritization. Framboidal, subhedral and microcrystalline are the predominant pyrite textures detected in the cells. Abundant pyritized vegetal debris have also been found inside the amber nuggets and the surrounding sediments. This vegetal debris usually contained numerous pyrite framboids and very densely packed polycrystalline pyrite formations infilled with different elements of the secondary xylem.ConclusionEmbedding in amber and pyritization are not always alternative modes of biological preservation during geological times, but double fossilization is possible under certain environmental conditions. Pyritization in protists shows a quite different pattern with regard to plants, due to the different composition and cellular architecture in these microorganisms and organisms. Anaerobic sulphate-reducing bacteria could play a crucial role in this microbial fossilization.

Keratin Coatings for Wool: Shrinkproofing and Nanoparticle Delivery

AbstractSummary: Wool fabrics were treated with keratin hydrolysate in isolated systems, in systems incorporating a cross‐linking enzyme, and in systems with nanoparticle silver. The dimensions of wool fabric were controlled after keratin applications and the strength of bleached wool fabric was improved. Keratin applications imparted these improved properties when applied alone and when applied with the enzyme. The enzyme was effective for in‐situ, solid‐state cross‐linking of wool fabric, cross‐linking keratin‐to‐keratin, and cross‐linking keratin‐to‐fabric. To further improve the properties of wool, nanoparticle silver was produced in various shapes. Transmission electron microscopy (TEM) micrographs of these particles showed discrete and isolated particles of size 8‐100 nm, dependent on the preparation. A combination of TEM and UV‐VIS spectroscopy was used to characterize these particles and scanning electron microscopy running in backscattered electron mode confirmed their placement on wool fibers. The application of nanoparticle silver to wool when co‐added with keratin may both improve dimensional stability and impart antimicrobial efficacy.

Deteriorating effects of lichen and microbial colonization of carbonate building rocks in the Romanesque churches of Segovia (Spain)

In this study, the deterioration effects of lichens and other lithobionts in a temperate mesothermal climate were explored. We examined samples of dolostone and limestone rocks with visible signs of biodeterioration taken from the exterior wall surfaces of four Romanesque churches in Segovia (Spain): San Lorenzo, San Martín, San Millán and La Vera Cruz. Biofilms developing on the lithic substrate were analyzed by scanning electron microscopy. The most common lichen species found in the samples were recorded. Fungal cultures were then obtained from these carbonate rocks and characterized by sequencing Internal Transcribed Spacers (ITS). Through scanning electron microscopy in back-scattered electron mode, fungi (lichenized and non-lichenized) were observed as the most frequent microorganisms occurring at sites showing signs of biodeterioration. The colonization process was especially conditioned by the porosity characteristics of the stone used in these buildings. While in dolostones, microorganisms mainly occupied spaces comprising the rock's intercrystalline porosity, in bioclastic dolomitized limestones, fungal colonization seemed to be more associated with moldic porosity. Microbial biofilms make close contact with the substrate, and thus probably cause significant deterioration of the underlying materials. We describe the different processes of stone alteration induced by fungal colonization and discuss the implications of these processes for the design of treatments to prevent biodeterioration.

Synthesis and properties of triangular-shaped GaN nanorods via growth mode control

The synthesis of wurtzite gallium nitride (GaN) nanorods with triangular shape on c-Al 2O 3 substrates using a thermal chemical vapor deposition process was investigated. It was possible to control nanorod shape and growth mode of GaN nanorods by change of sample geometry in the chamber using a mixture of GaN powder and Ga metal with ammonia gas reaction. It was found that the GaN nanorods were grown via both vapor–liquid–solid and vapor–solid mode with change of sample placement in the chamber. The morphology of the GaN nanorods was observed by field-emission scanning electron microscopy in secondary electron and back-scattered electron mode. High-resolution transmission electron microscopy, and X-ray scattering measurements revealed the GaN nanorods to have a single-crystalline wurtzite structure.

Does prism width from the shell prismatic layer have a random distribution?

A study of the distribution of the prism width inside the prismatic layer of Unio tumidus (Philipsson 1788, Diss Hist-Nat, Berling, Lundæ) from Lake Neuchâtel, Switzerland, has been conducted in order to determine whether or not this distribution is random. Measurements of 954 to 1,343 prism widths (depending on shell sample) have been made using a scanning electron microscope in backscattered electron mode. A white noise test has been applied to the distribution of prism sizes (i.e. width). It shows that there is no temporal cycle that could potentially influence their formation and growth. These results suggest that prism widths are randomly distributed, and related neither to external rings nor to environmental constraints.

Bioreceptivity of dolostones to fungal colonization

In many historic monuments in which signs of biodeterioration have been frequently reported, dolostones were used as dimension stone for their construction. In an effort to assess the influence of the texture of dolostones on their potential bioreceptivity, we characterized microbial colonization strategies in dolostone samples of predictably different textural features by scanning electron microscopy in back scattered electron mode (SEM-BSE), low temperature scanning electron microscopy (LTSEM), transmission light microscopy (TLM) and mercury intrusion porosimetry (MIP). Fungi were the predominant microorganisms in the dolostones examined and their colonization showed three well defined stages with the final consequence of complete rock disaggregation. The results of this study indicate that porosity differences (mainly the extent and type) were particularly relevant for determining the presence and extent of each colonization stage. As a determinant of bioreceptivity, the porosity of dolostones will also condition the decay processes associated with this colonization. These findings highlight the fact that the intrinsic properties of dolostones, such as texture, need to be considered when selecting this type of stone for future construction projects.

Effects of industrial by-product amendments on As, Cd and Tl retention/release in an element-spiked acidic soil

To asses the efficiency of two by-products (phosphogypsum (PG) and sugar foam (SF), rich in gypsum and calcium carbonate, respectively) in the immobilization of three toxic elements (As, Cd and Tl) in an acidic soil, batch-scale sorption and desorption experiments were conducted after 18 months of in situ amendment application. The Langmuir isotherms applied for sorption studies showed that the estimated maximum sorption capacity of the elements was highest in the SF-treated samples. The amount of element retained and the percentage of extraction after TCLP tests indicated that those samples amended with sugar foam (SF and PG + SF) had the potential to immobilize As, Cd and Tl in an acidic soil with low sorptive capacity. In addition to sorption and desorption experiments, scanning electron microscopy in back-scattered electron mode (SEM-BSE) showed the formation of Al-hydroxy polymers which provides the soil with additional sorption capacity. The three target elements were associated with the Al-hydroxy polymers, probably through direct coordination or the formation of ternary complexes. By means of statistical analysis it has been found that sorption processes of As, Cd and Tl in this soil mainly depend on the treatment, whereas desorption is an element-dependent process.

Recristalização do aço AISI 430 com estrutura colunar de grãos

O recozimento de materiais com grãos grosseiros permite observar importantes efeitos de orientação na recristalização. Amostras do aço inoxidável ferrítico AISI 430 estabilizado ao nióbio e com estrutura colunar de grãos foram deformadas até reduções de 50 e 80% e recozidas em temperaturas variando de 300 a 1100°C para avaliação do amolecimento e da cinética de recristalização. As amostras compreendem a seção longitudinal de uma placa obtida via lingotamento contínuo. A laminação foi realizada a morno (&lt;FONT FACE=Symbol&gt;»&lt;/FONT&gt; 480°C), numa configuração na qual os grãos colunares permaneceram alinhados com a direção normal (contornos de grão paralelos à DN). A caracterização microestrutural das amostras utilizou microscopia eletrônica de varredura (MEV) no modo de elétrons retroespalhados. Os resultados mostram que o tamanho de grão recristalizado varia localmente de região para região, indicando efeitos de orientação importantes.

Protein mapping of calcium carbonate biominerals by immunogold

The construction of metazoan calcium carbonate skeletons is finely regulated by a proteinaceous extracellular matrix, which remains embedded within the exoskeleton. In spite of numerous biochemical studies, the precise localization of skeletal proteins has remained for a long time as an elusive goal. In this paper, we describe a technique for visualizing shell matrix proteins on the surface of calcium carbonate crystals or within the biominerals. The technique is as follows: freshly broken pieces of biominerals or NaOCl then EDTA-etched polished surfaces are incubated with an antibody elicited against one matrix protein, then with a secondary gold-coupled antibody. After silver enhancement, the samples are subsequently observed with scanning electron microscopy by using back-scattered electron mode. In the present case, the technique is applied to a particular example, the calcitic prisms that compose the outer shell layer of the mediterranean fan mussel Pinna nobilis. One major soluble protein, caspartin, which was identified recently, was partly de novo sequenced after enzymatic digestions. A polyclonal antibody raised against caspartin was used for its localization within and on the prisms. The immunogold localization indicated that caspartin surrounds the calcitic prisms, but is also dispersed within the biominerals. This example illustrates the deep impact of the technique on the definition of intracrystalline versus intercrystalline matrix proteins. Furthermore, it is an important tool for assigning a putative function to a matrix protein of interest.

Development and Structure of Eukaryotic Biofilms in an Extreme Acidic Environment, Río Tinto (SW, Spain)

An in situ colonization assay was performed to study the early stages of biofilm formation in Rio Tinto (SW, Spain), an extremely acidic environment (pH ca. 2). Eukaryotic assemblages were monitored at monthly intervals for 1 year. Diversity, colonization rates, and seasonal variations were analyzed. Structural features of naturally grown biofilms were explored by light and scanning electron microscopy in backscattered electron mode. A total of 14 taxa were recognized as constituents of the eukaryotic assemblages. The eukaryotic communities were dissimilar at the different sampling sites. The lowest diversity was found at the most extreme locations, in terms of pH and heavy metal concentrations. The biofilms were mainly formed by species from the genera Dunaliella and Cyanidium. Two genera of filamentous algae, Zygnemopsis and Klebsormidium, were principally responsible for the variability in the cell number throughout the year. These species appear in June to decrease almost completely between October and November. In contrast, the number of heterotrophic flagellates and ciliates remained constant throughout the year. The microcolonization sequence showed an initial accumulation of amorphous particles composed of bacteria and inorganic grains of minerals. By the end of the second month, the organic matrix was also populated by fungi, bacteria, and a few eukaryotic heterotrophs such as amoebae and small flagellates. Diatoms only showed significant colonization in regions where mycelial matrices were first established. Flagellated green algae such as Dunaliella or Chlamydomonas as well as Euglena were also present at the very beginning of the biofilm development, although in low numbers (<100 cells cm(-2)). After the flagellated cells, sessile species of algae such Chlorella or Cyanidium appeared. Filamentous algae were the last species to colonize the biofilms. Most of the naturally grown biofilms were found to be structures composed of different species organized in different layers separated, probably by extracellular polymeric substances, although more analysis should be done in this regard. The possible implications of the biofilm structure in the adaptation to this extreme habitat are discussed.

Micromorphological characterization and lithification of microbial mats from the Ebro Delta (Spain).

The structural organization of microbial mats from the Ebro Delta (Spain) and their accretion and partial lithification processes were explored using scanning electron microscopy in back-scattered electron mode and low-temperature scanning electron microscopy. Two differentiated zones were distinguished in a transverse section of a fragment taken from the mat at a depth of 2.5 mm. The first consisted of an upper layer in which the dominant microorganisms, Microcoleus spp., actively grew in an embedded slack matrix of exopolysaccharides. Microcoleus filaments were oriented parallel to the surface and to each other, with filaments below arranged perpendicularly to one another but without crossing. Most of the minerals present were allochthonous grains of calcium phosphate biocorroded by cyanobacteria. The second zone was below a depth of 1 mm and made up of accretion layers with large deposits of calcium carbonate and smaller amounts of calcium phosphate of biological origin. The predominance of a particular type of mineral precipitation with a characteristic external shape and/or texture within a zone, e.g., sponge-like deposits of calcium phosphate, appears to depend on the taxa of the prevailing microorganisms.

Microstructural characterization of as-cast Co–B alloys

This work presents results of microstructural characterization of as-cast Co–B alloys. Samples of different compositions were prepared by arc melting Co (min. 99.97%) and B (min. 99.5%) under argon atmosphere in a water-cooled copper crucible with non-consumable tungsten electrode and titanium getter. All samples were characterized by scanning electron microscopy (SEM) in back-scattered electron (BSE) mode, X-ray diffraction (XRD) and wavelength dispersive spectrometry (WDS). A good agreement is observed between the obtained microstructures and those expected by the currently accepted Co–B phase diagram.

Qualitative analysis of adhesive interface nanoleakage using FE-SEM/EDS

Objectives The purpose of this study was to evaluate the quality of short term sealing of current adhesives. Methods Five adhesive systems were used and evaluated in this study; two kinds of two-step adhesives (Single Bond and Clearfil SE Bond) and three one-step adhesives (Clearfil S 3 Bond, G Bond and One-Up Bond F-plus). Flat occlusal superficial dentin surfaces from extracted human third molars were finished with wet 600-grit silicon-carbide paper and bonded with one of the adhesives. After 24 h storage at 37 °C in water, the bonded assemblies were sectioned into approximately 1 mm thick slabs. Two central slabs from each tooth were chosen and immersed into 50% (w/v) solution of silver ammoniacal nitrate for 18 h and exposed to photodeveloping solution for 6 h. The specimens were then slightly polished, argon ion-etched. In order to examine the nanoleakage within the resin/dentin interface, penetration of silver was observed in a field emission (FE)-SEM using yttrium–aluminium–garnet (YAG) backscattered electron mode. EDS analysis was also carried out in parallel to identify the existence of metallic silver particles. Results The penetration pattern of silver depended on the adhesive used, indicating different nanoleakage in different adhesive systems. Single Bond, One-Up Bond F-plus and G Bond showed clear silver uptake in both the adhesive and hybrid layer. Clearfil SE Bond showed less silver penetration and slight silver peak on the elemental energy spectroscopy of EDS. Clearfil S 3 Bond did not display clear silver penetration under 2000× magnification by FE-SEM, and no existence of metallic silver of the Clearfil S 3 Bond group by EDS, could be detected. Significance The nanoleakage, as well as its location depends on the adhesives. Different nanoleakage expressions were revealed between two-step and one-step adhesives and also among one-step adhesives themselves.

Microstructural characterization of as-cast Co–Si alloys

This work presents results of microstructural characterization of as-cast Co–Si alloys. The alloys of different compositions were prepared by arc melting Co (min. 99.97%) and Si (min. 99.99%) under argon atmosphere in a water-cooled copper crucible with a nonconsumable tungsten electrode and titanium getter. All samples were characterized by scanning electron microscopy (SEM) using back-scattered electron (BSE) mode and X-ray diffraction (XRD). A good conformity between the currently accepted Co–Si phase diagram and the experimental results from this work was verified. No indication of the βCo 2Si was observed in the as-cast microstructures. As in previous investigations, the Co 3Si phase has not been observed in the samples at room temperature; however, microstructural evidence suggests its stability at high temperature.

Biomineralization of endolithic microbes in rocks from the McMurdo Dry Valleys of Antarctica: implications for microbial fossil formation and their detection

In some zones of Antarctica's cold and dry desert, the extinction of cryptoendolithic microorganisms leaves behind inorganic traces of microbial life. In this paper, we examine the transition from live microorganisms, through their decay, to microbial fossils using in situ microscopy (transmission electron microscopy, scanning electron microscopy in back-scattered electron mode) and microanalytical (energy dispersive X-ray spectroscopy) techniques. Our results demonstrate that, after their death, endolithic microorganisms inhabiting Commonwealth Glacier sandstone from the Antarctica McMurdo Dry Valleys become mineralized. In some cases, epicellular deposition of minerals and/or simply filling up of empty moulds by minerals leads to the formation of cell-shaped structures that may be considered biomarkers. The continuous deposition of allochthonous clay minerals and sulfate-rich salts fills the sandstone pores. This process can give rise to microbial fossils with distinguishable cell wall structures. Often, fossilized cell interiors were of a different chemical composition to the mineralized cell walls. We propose that the microbial fossil formation observed was induced by mineral precipitation resulting from inorganic processes occurring after the death of cryptoendolithic microorganisms. Nevertheless, it must have been the organic template that provoked the diffusion of mineral elements and gave rise to their characteristic distribution pattern inside the fossilized cells.

Ultramorphological analysis of resin-dentin interfaces produced with water-based single-step and two-step adhesives: nanoleakage expression.

This study evaluated the nanoleakage patterns in bonded interfaces using two single-step, self-etching adhesives (Adper Prompt-AD, and One-up Bond F-OB), two two-step, self-etching primers (Clearfil SE Bond-CF, and Unifil Bond-UB), and one two-step, total-etch adhesive (Single Bond-SB). Dentin surfaces were bonded with the adhesive systems and stored in water at 37 degrees C for 1 week and 6 months. After storage periods, teeth were sectioned into 0.8 mm-thick slabs, coated with nail varnish except for the bonded interfaces, and immersed in ammoniacal AgNO(3) for 24 h. After immersion in photodeveloping solution, bonded sections were prepared and observed under a SEM using the backscattered electron mode. Undemineralized, unstained, epoxy resin-embedded sections were prepared for TEM. Nanoleakage patterns were qualitatively compared between periods. Nanoleakage was observed in all bonded specimens at both periods. CF and UB presented silver deposits predominantly restricted to the thin (0.5 microm) hybrid layer (HL) at both periods. Although no evident differences were observed in the nanoleakage pattern of UB at 7 days and 6 months, CF presented enlarged areas of silver impregnation after 6 months. SB presented accumulation of silver particles mostly within the HL at 7 days, which was intensified after 6 months. AD and OB presented massive silver accumulation within the HL and the overlying adhesive layer. No evident differences were noticed between storage periods. Silver impregnation increased for all adhesive systems from 7 days to 6 months, except for UB.