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.

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.

Characteristics of electron beam welded Ti & Ti alloys

Similar and dissimilar butt joint welds comprising combinations of commercially pure grade 4 titanium (CP-Ti), Ti-6Al-4V (Ti-64) and Ti-5Al-5V-5Mo-3Cr (Ti-5553) were created using the electron beam process. The resultant welds were studied by means of metallography, optical microscopy, mechanical testing and scanning electron microscopy. Mechanical testing was performed on welded samples to study the joint integrity and fracture characteristics. A scanning electron microscope investigation was performed on the fracture surface to reveal their fracture modes. While all weldments were crack free and most weldments exhibited mechanical properties comparable to the base metal, negligible ductility was exhibited during tensile testing joints of Ti- 5553 welded to either Ti-64 or Ti-5553.

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.

Wootz steel project by electron backscatter diffraction

The data is from an electron backscatter diffraction (EBSD) study of the microstructure of high carbon ‘Wootz’ steel. The objective of the study is to infer an unknown thermomechanical history from observation and analysis of the final microstructure in various ancient artefacts (swords and tools), and then compare the findings with heat treatments of the ancient artefacts and modern attempts at duplication of the structure. Electron backscatter data reveals the orientation relationships between various phases in the material, particularly cementite and ferrite. The dataset is randomly structured and organised. The data is automatically generated by an electron backscattered diffraction system attached to a field emission scanning electron microscope. The dataset uses proprietary software (cannot be copied or distributed without complying with licensing agreements): Oxford HKL Channel 5. As the native formats are binary they cannot be read with standard software.

Quantitative secondary electron imaging for work function extraction at atomic level and layer identification of graphene

Two-dimensional (2D) materials usually have a layer-dependent work function, which require fast and accurate detection for the evaluation of their device performance. A detection technique with high throughput and high spatial resolution has not yet been explored. Using a scanning electron microscope, we have developed and implemented a quantitative analytical technique which allows effective extraction of the work function of graphene. This technique uses the secondary electron contrast and has nanometre-resolved layer information. The measurement of few-layer graphene flakes shows the variation of work function between graphene layers with a precision of less than 10 meV. It is expected that this technique will prove extremely useful for researchers in a broad range of fields due to its revolutionary throughput and accuracy.

On the production of randomly-oriented recrystallization nuclei for selective growth experiments

The ideal starting condition for selective growth experiments is one having a layer of randomly-oriented nuclei adjacent to a matrix with negligible orientational variation but sufficient stored energy to promote growth. In practice, cutting or deformation processes are used in an attempt to approximate these ideal conditions, but the degree to which this is achieved has not been rigorously quantified. In this work, Fe-3wt%Si single crystals were cut or deformed using six different processes. The variation in texture with distance from the cut or deformed surface was measured using electron backscatter diffraction (EBSD) in a field emission gun scanning electron microscope (FEG-SEM) in order to assess the ability of each process to create conditions suitable for selective growth experiments. While grooving with a machine tool produced the best spread of orientations at the cut surface, the suitability of this process is diminished by the presence of a differently-textured deformed layer between the cut surface and the single crystal matrix. Grinding produced a less ideal distribution of orientations at the cut surface, but the presence of these orientations in a very thin layer adjacent to the matrix makes this process preferable for preparing crystals for selective growth experiments, provided the results are corrected for the deviation in the distribution of nuclei orientations from a random distribution.

Understanding the deformed microstructure of cold-rolled IF and LC steel

This paper presents an overview of a series of investigations of the microstructure and texture of cold-rolled IF and LC steel. The investigations made extensive use of orientation mapping using electron backscattered diffraction (EBSD) in a field emission gun scanning electron microscope (FEG-SEM). The effect of grain boundaries on the deformed microstructure was examined by comparing the textures of regions near grain boundaries and in the interiors of grains.  A general weakening of the texture, but a strengthening of the {OOI}<110> component, occurs in the vicinity of grain boundaries. Misorientation angle and axis distributions were used to characterise the fragmentation of grains belonging to different orientation classes. The influence of carbon on the deformed microstructure and nucleation during recrystallization was clarified by examining the microstructures of LC and IF steels during rolling and annealing. The
results of the investigations emphasize the important role of shear banding in determining the fragmentation behaviour of ND-fibre grains and the orientations of viable recrystallization nuclei within the deformed microstructure.

Polypyrrole nanoparticles and dye absorption properties

Polypyrrole (PPy) nanoparticles were prepared by using microemulsion polymerization processes at 3 °C. Particle characterization was performed by using FTIR, elementary analysis, UV–vis spectra and scanning electron microscope (SEM). The size of the nanoparticles varied from about 50 to 100 to 100 to 200 nm with the change in concentration of surfactant from 0.8 to 0.44 M. Polypyrrole nanoparticles were dedoped by a 10% NaOH solution, followed by a redoping process using a nuclear fast red kernechtrot dye, which has a sulfonate group. Dedoping changed the optical absorption properties of the nanoparticles.

Internal structure and pigment granules in colored alpaca fibers

Alpaca fibers have some distinct properties such as softness and warmth, which have not been fully understood in combination with the fiber internal structures. In the present investigation, the internal structures of alpaca fibers have been closely examined under the scanning electron microscope (SEM), especially in the longitudinal direction. The results showed that numerous pigment granules reside loosely inside pockets in brown and dark-brown alpaca fibers. These pigment granules were mainly distributed inside the cortical cells, the medullation regions as well as underneath the cuticles. Their size in the brown alpaca fibers was smaller and more uniformly round than in the dark-brown fibers. These granules in colored alpaca fibers loosen the bundle of cortical cells, providing many crannies in the fibers which may contribute to the superior flexibility, warmth and softness of the fibers. Moreover, there are no heavy metal elements found in the granules. The mordant hydrogen peroxide bleaching employed could eliminate the pigment granules and create many nano-volumes for further dyeing of fibers into more attractive colors.

Surface morphologies and internal fine structures of bast fibers

Fiber surface morphologies and associated internal structures are closely related to its properties. Unlike other fibers including cotton, bast fibers possess transverse nodes and fissures in cross-sectional and longitudinal directions. Their morphologies and associated internal structures were anatomically examined under the scanning electron microscope. The results showed that the morphologies of the nodes and the fissures of bast fibers varied depending on the construction of the inner fibril cellular layers. The transverse nodes and fissures were formed by the folding and spiralling of the cellular layers during plant growth. The dimensions of nodes and fissures were determined by the dislocations of the cellular layers. There were also many longitudinal fissures in bast fibers. Some deep longitudinal fissures even opened the fiber lumen for a short way along the fiber. In addition, the lumen channel of the bast fibers could be disturbed or disrupted by the nodes and the spirals of the internal cellular layers. The existence of the transverse nodes and fissures in the bast fibers could degrade the fiber mechanical properties, whereas the longitudinal fissures may contribute to the very rapid moisture absorption and desorption.

The determination of the local conditions for void initiation in front of a crack tip for materials with second-phase particles

A procedure is proposed to determine, for second-phase particles near a crack tip, the maximum particle stresses at the moment of void initiation by either particle fracture or particle/matrix interface separation. A digital image analysis system is applied to perform a quantitative analysis of corresponding fracture surface regions from stereo image pairs taken in the scanning electron microscope. The fracture surface analysis is used to measure, for individual particles, the crack tip opening displacement at the moment of void initiation and the particle location with respect to the crack tip. From these data, the stress tensor at the moment of void initiation is calculated from the Hutchinson–Rice–Rosengren (HRR) field theory. The corresponding average local stresses within the particle are evaluated by a non-linear Mori–Tanaka-type approach. These stresses are compared to estimates according to the models by Argon et al. [A.S. Argon, J. Im, R. Safoglu, Metall. Trans. 6 (1975) 825] and Beremin [F.M. Beremin, Metall. Trans. 12 (1981) 723]. The procedure is demonstrated on an Al6061–10% Al2O3 metal matrix composite.