A surface characterisation and microstructural study by scanning electron microscopy of the N-methyl-n-alkylpyrrolidinium tetrafluoroborate organic salts

A microstructural characterisation of the family of N-methyl-N-alkylpyrrolidinium tetrafluoroborate organic salts was carried out by observation of powder surface morphologies with the aim of extending the microstructure-property correlation. Inherent difficulties limiting extensive studies of organic solids by SEM, including volatility under vacuum, charging due to electron beam irradiation, and air-sensitivity were overcome with the use of a Field Emission SEM and cryostage attachment. This technique, providing considerable improvements in image quality at low accelerating voltages, enabled direct observation of complex microstructural features in samples exhibiting high temperature plastic crystalline phases (N,N-dimethylpyrrolidinium tetrafluoroborate [P11BF4]; N-methyl-N-ethylpyrrolidinium tetrafluoroborate [P12BF4]; N-methyl-N-propylpyrrolidinium tetrafluoroborate [P13BF4]). Extensive lattice imperfections including grain boundaries, slip planes and dislocation pits were observed within particles of approximately 200 mgrm diameter. The N-methyl-N-butylpyrrolidinium tetrafluoroborate (P14BF4) sample in this series revealed columnar single crystals with high aspect ratios. The origin of plastic flow properties is discussed using single crystal and polycrystalline slip observations and a relationship proposed between defect characteristics and transport properties.

Applications of scanning electrochemical microscopy (SECM) for local characterization of AZ31 surface during corrosion in a buffered media

Different modes of scanning electrochemical mapping (SECM) such as surface generation/tip collection (SG/TC), amperometry, AC-SECM and potentiometry were employed to characterize the active/passive domains, hydrogen gas (H2) evolution and local pH on a corroding surface of AZ31 in simulated biological fluid (SBF). It was found that the main domains of H2 evolution are associated with lower insulating properties of the surface as well as higher local pH. The near surface pH was found to be highly alkaline indicating that, even in a buffered solution such as SBF, the local pH on a corroding AZ31 surface can be significantly different to the bulk pH. © 2014 Elsevier Ltd.

Silver sulfide as a staining agent for scanning electron microscopy of nylon 6/MXD6 blends

BACKGROUND: In transmission and scanning electron microscopy imaging, the ability to obtain sufficient contrast between the components of a blend when they are both of a similar chemical structure still remains problematic. This paper investigates the domain morphology of a polymer blend containing two polyamides, nylon 6 and the semi-aromatic polyamide poly(m-xylene adipamide) (MXD6), using scanning electron microscopy in backscattered electron imaging mode. The efficiency of three staining agents, ruthenium tetroxide, phosphotungstic acid and silver sulfide, in obtaining optimum phase contrast between the two polymers is discussed.
RESULTS: The use of silver sulfide as a staining agent was found to be a fast and reliable approach which required basic sample preparation and provided excellent compositional contrast between the phases present in the nylon 6/MXD6 blends compared to the other staining agents.
CONCLUSIONS: The technique described in this paper is believed to be a novel and versatile method that has the potential to further improve the ability to study complex polymer blends where one polymer contains an aromatic ring.

Gold-nanorod-facilitated nonlinear optical microscopy under radially polarised beam illumination

Reports on the use of radially polarised beam in gold-nanorod-facilitated nonlinear microscopy and therapy. It has been found that the use of radially polarised beam can greatly reduce the energy fluence threshold for treating cancer cells labelled with gold nanorods. The slight distortion in the polarisation properties of the radially polarised beam after propagating through double-clad photonic crystal fibres makes it promising in the application of fibre-optic based endoscopic system.

Interfacing cell-based assays in environmental scanning electron microscopy using dielectrophoresis

Development of the dielectrophoretic (DEP) live cell trapping technology and its interfacing with the environmental scanning electron microscopy (ESEM) is described. DEP microelectrode arrays were fabricated on glass substrate using photolithography and lift-off. Chip-based arrays were applied for ESEM analysis of DEP-trapped human leukemic cells. This work provides proof-of-concept interfacing of the DEP cell retention and trapping technology with ESEM to provide a high-resolution analysis of individual nonadherent cells.

Measuring the adhesion force on natural fibre surface using scanning probe microscopy

This work has focused on measuring the adhesion forces on both untreated and atmospheric helium plasma treated single jute fibre surfaces using scanning probe microscopy (SPM). The measurements were conducted on three differently aged surfaces for one week, three weeks and six weeks using a standard silicon nitride tip in force-volume (f-v) mode. Up to 256 adhesion data points were collected from various locations on the surface of the studied fibres using in-house developed software and the resulting data were statistically analysed by the histogram method. Results obtained from this analysis method were found to be very consistent with a small statistical variation. The work of adhesion, Wa, was calculated from measured adhesion force using the Johnson–Kendall–Roberts (JKR) and Derjaguin–Muller–Toporov (DMT) models. Increases in both adhesion force and work of adhesion were observed on jute fibre with certain levels of atmospheric plasma treatment and ageing time.

High-temperature laser-scanning confocal microscopy as a tool to study the interface instability during unsteady-state solidification of low-carbon steel

Solidification microstructure is a defining link between production techniques and the mechanical properties of metals and in particular steel. Due to the difficulty of conducting solidification studies at high temperature, knowledge of the development of solidification microstructure in steel is scarce. In this study, a laser-scanning confocal microscopy (LSCM) has been used to observe in situ and in real-time the planar to cellular to dendritic transition of the progressing solid/liquid interface in low carbon steel. Because the in situ observations in the laser-scanning confocal microscopy are restricted to the surface, the effect of sample thickness on surface observations was determined. Moreover, the effect of cooling rate and alloy composition on the planar to cellular interface transition was investigated. In the low-alloyed, low-carbon steel studied, the cooling rate does not seem to have an effect on the spacing of the cellular microstructure. However, in the presence of copper and manganese, the cell spacing decreased at higher cooling rates. Higher concentrations of copper in steel resulted on an increased cell spacing at the same cooling rates.

Corrosion protection afforded by praseodymium conversion film on Mg alloy AZNd in simulated biological fluid studied by scanning electrochemical microscopy

Surface passivation of AZNd Mg alloy with Pr(NO3)3 is studied using scanning electrochemical microscopy (SECM) in surface generation/tip collection (SG/TC) and AC modes. Corrosion protection afforded by the Pr treatment and the degradation mechanism in a simulated biological environment was examined on a local scale and compared with non-treated AZNd. SG/TC mode results revealed a drastic decrease in H2 evolution due to the Pr treatment. Mapping the local insulating characteristics using AC-SECM showed higher conductivity of the surface where H2 evolution was most favorable.

Confocal laser scanning microscopy elucidation of the micromorphology of the leaf cuticle and analysis of its chemical composition

Electron microscopy techniques such as transmission electron microscopy (TEM) and scanning electron microscopy (SEM) have been invaluable tools for the study of the micromorphology of plant cuticles. However, for electron microscopy, the preparation techniques required may invariably introduce artefacts in cuticle preservation. Further, there are a limited number of methods available for quantifying the image data obtained through electron microscopy. Therefore, in this study, optical microscopy techniques were coupled with staining procedures and, along with SEM were used to qualitatively and quantitatively assess the ultrastructure of plant leaf cuticles. Leaf cryosections of Triticum aestivum (wheat), Zea mays (maize), and Lupinus angustifolius (lupin) were stained with either fat-soluble azo stain Sudan IV or fluorescent, diarylmethane Auramine O and were observed under confocal laser scanning microscope (CLSM). For all the plant species tested, the cuticle on the leaf surfaces could be clearly resolved in many cases into cuticular proper (CP), external cuticular layer (ECL), and internal cuticular layer (ICL). Novel image data analysis procedures for quantifying the epicuticular wax micromorphology were developed, and epicuticular waxes of L. angustifolius were described here for the first time. Together, application of a multifaceted approach involving the use of a range of techniques to study the plant cuticle has led to a better understanding of cuticular structure and provides new insights into leaf surface architecture.

Recrystallization textures in course grained low carbon and interstitial free steels

The microstructures and textures of coarse grained cold rolled, partially recrystallized and fully recrystallized low carbon and interstitial free steel were examined by optical microscopy, scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD). The recrystallization textures of the two grades are markedly different, with the low carbon steel having a predominantly Goss {11O}<OOl> texture and the interstitial free steel having a <1ll>/1ND texture with a strong {III }<112> component. One possible explanation for the texture difference is that less severe localization of flow during deformation of interstitial free steels causes less Goss nuclei to be generated. While some support for this view is provided by the results presented in this paper, the results suggest that another mechanism may be at least partially responsible. Examination of micro
shear bands on the surface of pre-polished samples showed that a higher proportion of micro shear bands remained active at high rolling reductions in the low carbon steel, compared with the interstitial free grade. Regions of Goss orientation within bands that have ceased to operate rotate to
near-{ III }<112> orientations with further deformation. Consequently, the recrystallization texture of coarse grained interstitial free steels can be rationalized by a reduction in the availability of Goss nuclei and an increase in the availability of {Ill }<112> nuclei due to a "Goss to {Ill }<112>" rotation within micro shear bands that have ceased to operate.

Correlation between optical and SEM measurements of wool cortical cell size

Wool fibres consist of micro to nano scale protein constituents that could be used for innovative applications. While techniques for extracting these constituents or making wool fibres into organic powders have been developed, effectively dispersing the particles and accurately determining their size has been difficult in practice. In this study, an ultrasonic method was employed to disperse cortical cells extracted from wool fibres into an
immersion oil or ethanol. Specimens of the cortical cells were then observed under optical microscopy and scanning electron microscopy, respectively. Cell length and maximum cell diameter were measured to quantify the cell size. The results suggest significant discrepancies exist in the cortical cell size obtained from the two different measurement techniques. The maximum diameter of wool cortical cells obtained from the optical microscope was much larger than that from the scanning electron microscope, while the length was much shorter. A correction factor is given so that cortical cell size obtained from the two measurement techniques can be compared.

Controlled synthesis and characterization of 10 nm thick Al2O3 nanowires

α-Al₂O₃ nanowires, with diameter around 10 nm, were synthesized in bulk quantity by heating the mixture of pure aluminum and graphite powders at 900 °C. Scarcity of oxygen is regarded as the reason for the growth of the small diameter α-Al₂O₃ nanowires at relatively low temperature. The product was characterized by field emission scanning electron microscopy, high-resolution transmission electron microscopy and photoluminescence. The Oxygen vacancies in the nanowires lead to the strong photoluminescence in the wavelength range of 400–700 nm with its peak at 527 nm.