Optical, electrochemical and morphological investigations of poly (3,4-propylenedioxythiophene)-sultone (PProDOT-S) thin films

In this paper, we have carried out thin film characterization of poly(3,4-propylenedioxythiophene)-sultone (PProDOT-S), a derivative of electrochromic poly(3,4-propylenedioxythiophene) (PProDOT). PProDOT-S was deposited onto transparent conducting oxide coated glass substrates by solution casting method. Single wavelength spectrophotometry is used to monitor the switching speed and contrast ratio at maximum wavelength (lambda (max)). The percentage transmittance at the lambda (max) of the neutral polymer is monitored as a function of time when the polymer film is repeatedly switched. This experiment gives a quantitative measure of the speed with which a film is able to switch between the two states i.e. the coloured and the bleached states. PProDOT-S films were switched at a voltage of 1 center dot 9 V with a switching speed of 2 s at lambda (max) of 565 nm and showed a contrast of similar to 37%. Cyclic voltammetry performed at different scan rates have shown the characteristic anodic and cathodic peaks. The structural investigations of PProDOT-S films by IR spectra were in good agreement with previously reported results. Raman spectra of PProDOT-S showed a strong Raman peak at 1509 cm (-aEuro parts per thousand 1) and a weak peak at 1410 cm (-aEuro parts per thousand 1) due to the C = C asymmetric and symmetric stretching vibrations of thiophene rings. The morphological investigations carried out by using scanning electron microscope (SEM) of polymer films have shown that these polymers are found to be arranged in dense packed clusters with non-uniform distribution having an average width and length of 95 nm and 160 nm, respectively.

Preliminary Investigations on Low-Pressure Laminar Plasma Spray Processing

The usual plasma spraying methods often involve entrainment of the surrounding air into the turbulent plasma core and result in coated materials having relatively high porosity and low adhesive strength. Therefore, exploration of new plasma spraying methods for fabricating high quality coatings to meet the requirement of special applications will be quite important. In this study, an alternative plasma spraying method, i.e. the low-pressure laminar plasma spraying process, is investigated and used in an attempt for spraying thermal barrier coatings (TBCs). Investigations on the characteristics of the laminar plasma jets, feeding methods for the ceramic powder and the formation process of the individual quenched splats have been carried out. The properties of the TBCs sprayed by laminar plasma jet process, such as the adhesive strength at the interface of the ceramic coating/bond coat, the surface roughness and microstructure, are examined by tensile tests and scanning electron microscope (SEM) observations.

Transmission electron microscopy of marine crustacean eggs

Ultrastructural investigations of eggs can be important in helping to understand embryonic development. There are few transmission electron microscope studies of marine arthropod eggs, however, as they have proved difficult to fix and infiltrate with resin. Here, we describe a modification of a standard method that allows the preparation of the quite different eggs of the marine copepod, Acartia tonsa and the lobster, Homarus gammarus, for transmission electron microscopy. By using double fixation and an extended resin infiltration time we obtained good preparations for electron microscopy. We anticipate that these modifications to the standard protocol will be widely applicable and useful for the study of the eggs and early developmental stages of many marine arthropod taxa. Les recherches sur l'ultrastructure des oeufs peuvent être importantes en aidant à comprendre le développement embryonnaire. Il existe cependant peu d'études en microscopie électronique à transmission sur les oeufs d'arthropodes marins, car il est difficile de les fixer et d'y infiltrer de la résine. Dans ce travail, nous décrivons une modification de la méthode standard, qui permet la préparation pour la microscopie électronique à transmission d'oeufs aussi différents que ceux du copépode marin Acartia tonsa et du homard Homarus gammarus. En utilisant une double fixation et un temps plus long d'infiltration de la résine, nous avons obtenu de bonnes préparations pour la microscopie électronique. Nous prévoyons que ces modifications du protocole standard seront largement applicables et utiles pour l'étude des oeufs et des premiers stades de développement de nombreux taxons d'arthropodes marins.

Efficient but destructive: a test of the dental wash technique using secondary electron microscopy

The Boyadjian et al dental wash technique provides, in certain contexts, the only chance to analyze and quantify the use of plants by past populations and is therefore an important milestone for the reconstruction of paleodiet. With this paper we present recent investigations and results upon the influence of this method on teeth. A series of six teeth from a three thousand years old Brazilian shellmound (Jabuticabeira II) was examined before and after dental wash. The main focus was documenting the alteration of the surfaces and microstructures. The status of all teeth were documented using macrophotography, optical light microscopy, and atmospheric Secondary Electron Microscopy (aSEM) prior and after applying the dental wash technique. The comparison of pictures taken before and after dental wash showed the different degrees of variation and damage done to the teeth but, also, provided additional information about microstructures, which have not been visible before. Consequently we suggest that dental wash should only be carried out, if absolutely necessary, after dental pathology, dental morphology and microwear studies have been accomplished. (C) 2010 Elsevier Ltd. All rights reserved.

Size-selective investigations of spectral and emission properties of small particles and nanotubes

In dieser Arbeit wurde die Elektronenemission von Nanopartikeln auf Oberflächen mittels spektroskopischen Photoelektronenmikroskopie untersucht. Speziell wurden metallische Nanocluster untersucht, als selbstorganisierte Ensembles auf Silizium oder Glassubstraten, sowie ferner ein Metall-Chalcogenid (MoS2) Nanoröhren-Prototyp auf Silizium. Der Hauptteil der Untersuchungen war auf die Wechselwirkung von fs-Laserstrahlung mit den Nanopartikeln konzentriert. Die Energie der Lichtquanten war kleiner als die Austrittsarbeit der untersuchten Proben, so dass Ein-Photonen-Photoemission ausgeschlossen werden konnte. Unsere Untersuchungen zeigten, dass ausgehend von einem kontinuierlichen Metallfilm bis hin zu Clusterfilmen ein anderer Emissionsmechanismus konkurrierend zur Multiphotonen-Photoemission auftritt und für kleine Cluster zu dominieren beginnt. Die Natur dieses neuen Mechanismus` wurde durch verschiedenartige Experimente untersucht. Der Übergang von einem kontinuierlichen zu einem Nanopartikelfilm ist begleitet von einer Zunahme des Emissionsstroms von mehr als eine Größenordnung. Die Photoemissions-Intensität wächst mit abnehmender zeitlicher Breite des Laserpulses, aber diese Abhängigkeit wird weniger steil mit sinkender Partikelgröße. Die experimentellen Resultate wurden durch verschiedene Elektronenemissions-Mechanismen erklärt, z.B. Multiphotonen-Photoemission (nPPE), thermionische Emission und thermisch unterstützte nPPE sowie optische Feldemission. Der erste Mechanismus überwiegt für kontinuierliche Filme und Partikel mit Größen oberhalb von mehreren zehn Nanometern, der zweite und dritte für Filme von Nanopartikeln von einer Größe von wenigen Nanometern. Die mikrospektroskopischen Messungen bestätigten den 2PPE-Emissionsmechanismus von dünnen Silberfilmen bei „blauer“ Laseranregung (hν=375-425nm). Das Einsetzen des Ferminiveaus ist relativ scharf und verschiebt sich um 2hν, wenn die Quantenenergie erhöht wird, wogegen es bei „roter“ Laseranregung (hν=750-850nm) deutlich verbreitert ist. Es zeigte sich, dass mit zunehmender Laserleistung die Ausbeute von niederenergetischen Elektronen schwächer zunimmt als die Ausbeute von höherenergetischen Elektronen nahe der Fermikante in einem Spektrum. Das ist ein klarer Hinweis auf eine Koexistenz verschiedener Emissionsmechanismen in einem Spektrum. Um die Größenabhängigkeit des Emissionsverhaltens theoretisch zu verstehen, wurde ein statistischer Zugang zur Lichtabsorption kleiner Metallpartikel abgeleitet und diskutiert. Die Elektronenemissionseigenschaften bei Laseranregung wurden in zusätzlichen Untersuchungen mit einer anderen Anregungsart verglichen, der Passage eines Tunnelstroms durch einen Metall-Clusterfilm nahe der Perkolationsschwelle. Die elektrischen und Emissionseigenschaften von stromtragenden Silberclusterfilmen, welche in einer schmalen Lücke (5-25 µm Breite) zwischen Silberkontakten auf einem Isolator hergestellt wurden, wurden zum ersten Mal mit einem Emissions-Elektronenmikroskop (EEM) untersucht. Die Elektronenemission beginnt im nicht-Ohmschen Bereich der Leitungsstrom-Spannungskurve des Clusterfilms. Wir untersuchten das Verhalten eines einzigen Emissionszentrums im EEM. Es zeigte sich, dass die Emissionszentren in einem stromleitenden Silberclusterfilm Punktquellen für Elektronen sind, welche hohe Emissions-Stromdichten (mehr als 100 A/cm2) tragen können. Die Breite der Energieverteilung der Elektronen von einem einzelnen Emissionszentrum wurde auf etwa 0.5-0.6 eV abgeschätzt. Als Emissionsmechanismus wird die thermionische Emission von dem „steady-state“ heißen Elektronengas in stromdurchflossenen metallischen Partikeln vorgeschlagen. Größenselektierte, einzelne auf Si-Substraten deponierte MoS2-Nanoröhren wurden mit einer Flugzeit-basierten Zweiphotonen-Photoemissions-Spektromikroskopie untersucht. Die Nanoröhren-Spektren wiesen bei fs-Laser Anregung eine erstaunlich hohe Emissionsintensität auf, deutlich höher als die SiOx Substratoberfläche. Dagegen waren die Röhren unsichtbar bei VUV-Anregung bei hν=21.2 eV. Eine ab-initio-Rechnung für einen MoS2-Slab erklärt die hohe Intensität durch eine hohe Dichte freier intermediärer Zustände beim Zweiphotonen-Übergang bei hν=3.1 eV.

Radial-field magnetic electron lenses

This investigation looks critically at conventional magnetic lenses in the light of present-day technology with the aim of advancing electron microscopy in its broadest sense. By optimising the cooling arrangements and heat transfer characteristics of lens windings it was possible to increase substantially the current density in the winding, and achieve a large reduction in the size of conventional magnetic electron lenses. Following investigations into the properties of solenoidal lenses, a new type of lens with only one pole-piece was developed. The focal properties of such lenses, which differ considerably from those.of conventional lenses, have been derived from a combination of mathematical models and experimentally measured axial flux density distributions. These properties can be profitably discussed with reference to "half-lenses". Miniature conventional twin pole-piece lenses and the proposed radial field single pole-piece lenses have been designed and constructed and both types of lenses have been evaluated by constructing miniature electron optical columns. A miniature experimental transmission electron microscope (TEM), a miniature scanning electron microscope (SEM) and a scanning transmission microscope (STEM) have been built. A single pole-piece miniature one million volt projector lens of only lOcm diameter and weighing 2.lkg was designed, built and tested at 1 million volts in a commercial electron microscope. iii. Preliminary experiments indicate that in single pole lenses it is possible to extract secondary electrons from the specimen in spite of the presence of the magnetic field of the probe-forming lens. This may well be relevant for the SEM in which it is desirable to examine a large specimen at a moderately good resolution.

In Situ Observation of the Thermal Decomposition of Weddelite by Heating Stage Environmental Scanning Electron Microscopy

The morphological and chemical changes occurring during the thermal decomposition of weddelite, CaC2O4·2H2O, have been followed in real time in a heating stage attached to an Environmental Scanning Electron Microscope operating at a pressure of 2 Torr, with a heating rate of 10 °C/min and an equilibration time of approximately 10 min. The dehydration step around 120 °C and the loss of CO around 425 °C do not involve changes in morphology, but changes in the composition were observed. The final reaction of CaCO3 to CaO while evolving CO2 around 600 °C involved the formation of chains of very small oxide particles pseudomorphic to the original oxalate crystals. The change in chemical composition could only be observed after cooling the sample to 350 °C because of the effects of thermal radiation.

Infrared spectra of Mg-SiO smokes : comparison with analytical electron microscopy studies

An important component of current models for interstellar and circumstellar evolution is the infrared (IR)spectral data collected from stellar outflows around oxygen-rich stars and from the general interstellar medium [1]. IR spectra from these celestial bodies are usually interpreted as showing the general properties of sub-micron sized silicate grains [2]. Two major features at 10 and 20 microns are reasonably attributed to amorphous olivine or pyroxene (e.g. Mg2Si04 or MgSi03) on the basis of comparisons with natural standards and vapor condensed silicates [3-6]. In an attempt to define crystallisation rates for spectrally amorphous condensates, Nuth and Donn [5] annealed experimentally produced amorphous magnesium silicate smokes at 1000K. On analysing these smokes at various annealing times, Nuth and Donn [5] showed that changes in crystallinity measured by bulk X-ray diffraction occured at longer annealing times (days) than changes measured by IR spectra (a few hours). To better define the onset of crystallinity in these magnesium silicates, we have examined each annealed product using a JEOL 1OOCX analytical electron microscope (AEM). In addition, the development of chemical diversity with annealing has been monitored using energy dispersive spectroscopy of individual grains from areas <20nm in diameter. Furthermore, the crystallisation kinetics of these smokes under ambient, room temperature conditions have been examined using bulk and fourier transform infrared (FTIR)spectra.

Electron petrography of fine-grained matrix in the Karoonda C4 carbonaceous chondrite

The study of matrices of rare Type 4 carbonaceous chondrites can reveal important information on parent body rnetamorp~ic processes and provide a comparison with processes on parent bodies of ordinary chc-idrites. Reflectance spectra (Tholen, 1984) from the two largest asteroids in the asteroid belt, Ceres and Pallas, suggest that they may be metamorphosed carbonaceous chondrites. These two asteroids constitute - onethird of the mass in the asteroid belt implying that type 4-6 carbonaceous chondrites are poorly represented in the meteorite collection and may be of considerable importance. The matrix of the C4 chondrite Karoonda has been investigated using a JEOL 2000FX analytical electron microscope (AEM) with an attached Tracor-Northem TN5500 energy dispersive spectrometer (EDS). In previous studies (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969), the petrography of the Karoonda matrix has been described as consisting largely of coarse-grained (50-200 urn in size) olivine and plagioclase (20-100 um in size), associated with micrometer sized magnetite and rare sulphides. AEM observations on matrix show that in addition to these large grains, there is a significant fraction (10 vol%) of interstitial fine grained phases « 5 urn). The mineralogy of these fine-grained phases differs in some respects from that of the coarser-grained matrix identified by optical and SEM techniques (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969). I~ particular crystals of two compositionally distinct pyroxenes « 2 urn in size) have been identified which have not been previously observed in Karoonda by other analytical techniques. Thin film microanalyses (Mackinnon et al., 1986) of these two pyroxenes indicate compositions consistent with augite and low-Ca pyroxene (- Fs27). Fine-grained anhedral olivine « 2 urn size) is the most abundant phase with composition -Fa29' This composition is essentially indistinguishable from that determined for coarser-grained matrix olivines using an electron microprobe (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969). All olivines are associated with subhedral magnetites « 1 urn size) which contain significant Cr (- 2%) and Al (- 1%) as was also noted for larger sized Karoonda magnetites by Delaney et al. (1985). It has recently been suggested (Burgess et al., 1987) on the basis of sulphur release profiles for S-isotope analyses of Karoonda that CaS04 (anhydrite) may be present. However, no sulphate phase has, as yet, been identified in the matrix of Karoonda. Low magnification contrast images suggest that Karoonda may have a significant porosity within the fine-grained matrix fraction. Most crystals are anhedral and do not show evidence for significant compaction. Individual grains often show single point contact with other grains which result in abundant intergranular voids. These voids frequently contain epoxy which was used as part of the specimen preparation procedure due to the friable nature of the bulk sample.

Electron microscopy of stratospheric particles

A recent NASA program to collect stratospheric dust particles using high-flying WB57 aircraft has made available many more potential candidates for the study of extraterrestrial materials. This preliminary report provides an interpretation of the types of particles returned from one flag (W7017) collected in August, 1981 using a subset of 81 allocated particles. This particular collection period is after the Mt. St. Helen's eruptions. Therefore, the flag may contain significant quantities of volcanic debris in addition to the expected terrestrial contaminants [1]. All particles were mounted on nucleopore filters and have been examined using a modified JEOL100CX analytical electron microscope. For most of the particles, X-ray energy dispersive spectra and images were obtained at 40kV on samples which have not received any conductive coating. However, in order to improve resolution (to ~30A) some images are recorded at 100kV. In addition, 16 samples have been coated with a thin layer (<50A) of Au/Pd.

Scanning electron microscopic study of microstructure of Gala apples during hot air drying

Microscopic changes occur in plant food materials during drying significantly influence the macroscopic properties and quality factors of the dried food materials. It is very critical to study microstructure to understand the underlying cellular mechanisms to improve performance of the food drying techniques. However, there is very limited research conducted on such microstructural changes of plant food material during drying. In this work, Gala apple parenchyma tissue samples were studied using a scanning electron microscope for gradual microstructural changes as affected by temperature, time and moisture content during hot air drying at two drying temperatures: 57 ℃ and 70 ℃. For fresh samples, the average cellular parameter values were; cell area: 20000 μm2, ferret diameter: 160 μm, perimeter: 600 μm, roundness: 0.76, elongation: 1.45 and compactness: 0.84. During drying, a higher degree of cell shrinkage was observed with cell wall warping and increase in intercellular space. However, no significant cell wall breakage was observed. The overall reduction of cell area, ferret diameter and perimeter were about 60%, 40% and 30%. The cell roundness and elongation showed overall increments of about 5% and the compactness remained unchanged. Throughout the drying cycle, cellular deformations were mainly influenced by the moisture content. During the initial and intermediate stages of drying, cellular deformations were also positively influenced by the drying temperature and the effect was reversed at the final stages of drying which provides clues for case hardening of the material.

Growth and electron effective mass measurements of strained Si and Si0.94Ge0.06 on relaxed Si0.62Ge0.38 buffers grown by rapid thermal chemical vapor deposition

Abstract: We report the growth and the electron cyclotron resonance measurements of n-type Si/Si0.62Ge0.38 and Si0.94Ge0.06/Si0.62Ge0.38 modulation-doped heterostructures grown by rapid thermal chemical vapor deposition. The strained Si and Si0.94Ge0.06 channels were grown on relaxed Si0.62Ge0.38 buffer layers, which consist of 0.6 mu m uniform Si0.62Ge0.38 layers and 0.5 mu m compositionally graded relaxed SiGe layers from 0 to 38% Ge. The buffer layers were annealed at 800 degrees C for 1 h to obtain complete relaxation. A 75 Angstrom Si(SiGe) channel with a 100 Angstrom spacer and a 300 Angstrom 2 X 10(19) cm(-3) n-type supply layer was grown on the top of the buffer layers. The cross-sectional transmission electron microscope reveals that the dense dislocation network is confined to the buffer layer, and relatively few dislocations terminate on the surface. The plan-view image indicates the threading dislocation density is about 4 X 10(6) cm(-2). The far-infrared measurements of electron cyclotron resonance were performed at 4 K with the magnetic field of 4-8 T. The effective masses determined from the slope of the center frequency of the absorption peak versus applied magnetic field plot are 0.203m(0) and 0.193m(0) for the two dimensional electron gases in the Si and Si0.94Ge0.06 channels, respectively. The Si effective mass is very close to that of a two dimensional electron gas in an Si MOSFET (0.198m(0)). The electron effective mass of Si0.94Ge0.06 is reported for the first time and is about 5% lower than that of pure Si.

In situ transmission electron microscopy study of deformation of an aluminum alloy tribolayer

Nanoscale deformation in the tribolayer of an Al–Mg alloy is studied using an in situ mechanical probe in a transmission electron microscope. The sample is strained locally at room temperature and the deformation is observed in real time. It is observed that when the tungsten probe comes into contact with the tribolayer, the material exhibits further hardening followed by material removal.

Comparative studies on the invasion of cattle ticks (Rhipicephalus (Boophilus) microplus) and sheep blowflies (Lucilia cuprina) by Metarhizium anisopliae (Sorokin).

Microscopic investigations over time were carried out to study and compare the pathogenesis of invasion of ticks and blowflies by Metarhizium anisopliae. The scanning electron microscope and stereo light microscope were used to observe and record processes on the arthropods' surfaces and the compound light microscope was used to observe and record processes within the body cavities. Two distinctly different patterns of invasion were found in ticks and blowflies. Fungal conidia germinated on the surface of ticks then hyphae simultaneously penetrated into the tick body and grew across the tick surface. There was extensive fungal degradation of the tick cuticle, particularly the outer endocuticle. Although large numbers of conidia adhered to the surface of blowflies, no conidia were seen to germinate on external surfaces. A single germinating conidium was seen in the entrance to the buccal cavity. Investigations of the fly interior revealed a higher density of hyphal bodies in the haemolymph surrounding the buccal cavity than in haemolymph from regions of the upper thorax. This pattern suggests that fungal invasion of the blowfly is primarily through the buccal cavity. Plentiful extracellular mucilage was seen around the hyphae on tick cuticles, and crystals of calcium oxalate were seen amongst the hyphae on the surface of ticks and in the haemolymph of blowflies killed by M. anisopliae isolate ARIM16.

Spinodal Decomposition in Tellurite-Based Glasses Induced by Excimer Laser Irradiation

Tellurite-based glasses in the TeO2-K3Li2Nb5O15, TeO2-Ba5Li2Ti2Nb8O30, and V2Te2O9 were fabricated by the conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via the X-ray powder diffraction technique and differential thermal analysis, respectively. The as-quenched samples were irradiated by an excimer laser (248 nm). The effect of laser power, duration of irradiation, and the frequency of the laser pulses on the surface features of the above glasses were studied. The optical microscopic studies carried out on the above systems revealed the presence of quasi-periodic and periodic structures on their surfaces. The local compositional variations of these structures were confirmed by back-scattered electron imaging using scanning electron microscope accompanied by energy-dispersive X-ray analysis. These results were convincing enough to state that the glasses in the present investigations had undergone spinodal decomposition on laser irradiation. The incidence of the interconnected texture of two different phases was observed owing to the quenching effect produced by the heating and cooling cycle of the successive laser pulses. Ring- and line-shaped patterns were also observed, respectively, when the pulse frequency of the laser and the duration of irradiation were increased.