The application of EDXS to the biological sciences

The distribution of chemical elements in soft tissues may be faithfully preserved by very rapid freezing. Most often the material is then cryosectioned and the sections frozen-dried prior to analysis, but direct analysis in the hydrated state is an established alternative. For bulk specimens, the shape of the analysed volume is uncertain. But whichever current model is accepted, analytical spatial resolution must generally be limited to the order of 1 μm. Such specimens can be suitable for the specific analysis of cytoplasm, cell nuclei and large extracellular spaces but not for study on a finer scale. Analytical spatial resolution in the range 200–500 nm is obtainable with sections cut ～ 1 μm thick. In the frozen-hydrated state, small extracellular spaces can be analysed but multiple scattering obscures intracellular detail in the STEM image. The irradiation required for an EDXS analysis, approximately 50 nanoCoulomb (50 nanoAmpere seconds), need not produce intolerable radiation damage when spread over an area 200 nm or more in diameter. Finer structure, for example mitochondria and regions of rough or smooth endoplasmic reticulum, can be identified and analysed in frozen-dried cryosections cut ～ 100 nm thick. Recently such features have been visualized in 100 nm frozen-hydrated sections where the water is vitreous. This opens the prospect of analysing material where elemental distributions have been preserved on a very fine scale, since one might avoid even the ionic shifts from aqueous solution to supramolecular structures which must occur on freeze-drying. But radiation damage may be prohibitive when an irradiation of 50 nanoCoulomb is concentrated into a hydrated area less than 200 nm in diameter.     

Chemical reactions and morphological stability at the Cu/Al2O3 interface

The microstructures of diffusion‐bonded Cu/(0001)Al₂O₃ bicrystals annealed at 1000 °C at oxygen partial pressures of 0.02 or 32 Pa have been studied with various microscopy techniques ranging from optical microscopy to high‐resolution transmission electron microscopy. The studies revealed that for both oxygen partial pressures a 20–35 nm thick interfacial CuAlO₂ layer formed, which crystallises in the rhombohedral structure. However, the CuAlO₂ layer is not continuous, but interrupted by many pores. In the samples annealed in the higher oxygen partial pressure an additional reaction phase with a needle‐like structure was observed. The needles are several millimetres long, ～10 µm wide and ～1 µm thick. They consist of CuAlO₂ with alternating rhombohedral and hexagonal structures. Solid‐state contact angle measurements were performed to derive values for the work of adhesion. The results show that the adhesion is twice as good for the annealed specimen compared to the as‐bonded sample.     

The Effect of Phosphazene additives to passivate and stabilize lubricants at the head/disk interface

There have been a number of applications for lubricant additives in the disk drive media area, the first of which was for pseudo-contact recording with inductive heads (tri-pad sliders) in an effort to stabilize the head/disk interface and minimize lube decomposition under hot/wet conditions. A number of additives have been tried which include antioxidants as well as Lewis bases, the latter in an effort to passivate the catalytic activity of the Lewis Acid sites on the slider which results in the decomposition of the perfluoropolyether (PFPE) lubricants such as Z-Dol, AM and Z-Tetraol. In addition to this passivation action of the phosphazene toward catalytic decomposition of the lubricant, it has recently been reported that the use of X-1P (a cyclic phosphazene) also enhances reflow of the lube, increasing the durability of the head disk interface. In this regard there are still a number of unanswered questions that pertain to the mechanism of the interaction of the X-1P with the lubricant and/or carbon to cause this increase in mobility of the lubricant resulting in the enhanced durability.There are numerous technical issues associated with the use of the various additives with the main one being compatibility between the additive and the PFPEs as well as the carbon surfaces on which they are coated. These issues include bonding, phase separation of the components, and the transfer mechanism for the additive to the slider where the passivation is required.In this paper, we will look at the interaction of the X-1P with the carbon overcoat on the media in an effort to try to better understand the mechanism of such an interaction and its effect on the mobility of the lubricant as well as the amount of bonded lube on the disks.     

Characterization of friction properties at the workmaterial/cutting tool interface during the machining of randomly structured carbon fibers reinforced polymer with carbide tools under dry conditions

Carbon fiber reinforced polymers (CFRP) are increasingly employed within the aerospace industry, particularly within the aircraft sector. However, machining of fiber reinforced composites can be quite complex, first due to the inherent heterogeneity resulting from the reinforcements/matrix assembly and second due to the presence of high modulus/high strength fibers. Therefore, a lot of Finite Element models have been developed in order to understand their material removal mechanisms. Among the scientific issues faced by these works, the identification of friction coefficients between CFRP and cutting tool materials remains a strategic field of research. This paper aims at characterizing the friction properties between composite and cutting tool materials. More precisely, the paper focuses on the context of a randomly structured CFRP, called HEXTOOL™, machined with a carbide tool under dry conditions. The specific tribological conditions during machining of such heterogeneous materials are discussed in the paper, especially the configuration of the tribosystem (‘opened tribosystem’). The great lack of friction coefficient is mainly due to the absence of relevant tribometers simulating the tribological conditions occurring in cutting. This paper presents the development of a new tribometer designed to simulate conditions corresponding to machining of randomly structured CFRP materials. It provides quantitative values of friction coefficient and heat partition coefficient depending on sliding velocities. This work has revealed that friction coefficients are very low in dry regime compared to those obtained in metal cutting. Moreover, experimental results confirm that friction coefficient decreases from 0.25 to 0.1 when sliding velocity increases. Finally this works establishes that a TiN layer deposited on carbide tools is not able to modify friction properties.     

Characterization of friction properties at the workmaterial/cutting tool interface during the machining of randomly structured carbon fibers reinforced polymer with carbide tools under dry conditions

Carbon fiber reinforced polymers (CFRP) are increasingly employed within the aerospace industry, particularly within the aircraft sector. However, machining of fiber reinforced composites can be quite complex, first due to the inherent heterogeneity resulting from the reinforcements/matrix assembly and second due to the presence of high modulus/high strength fibers. Therefore, a lot of Finite Element models have been developed in order to understand their material removal mechanisms. Among the scientific issues faced by these works, the identification of friction coefficients between CFRP and cutting tool materials remains a strategic field of research. This paper aims at characterizing the friction properties between composite and cutting tool materials. More precisely, the paper focuses on the context of a randomly structured CFRP, called HEXTOOL™, machined with a carbide tool under dry conditions. The specific tribological conditions during machining of such heterogeneous materials are discussed in the paper, especially the configuration of the tribosystem (‘opened tribosystem’). The great lack of friction coefficient is mainly due to the absence of relevant tribometers simulating the tribological conditions occurring in cutting. This paper presents the development of a new tribometer designed to simulate conditions corresponding to machining of randomly structured CFRP materials. It provides quantitative values of friction coefficient and heat partition coefficient depending on sliding velocities. This work has revealed that friction coefficients are very low in dry regime compared to those obtained in metal cutting. Moreover, experimental results confirm that friction coefficient decreases from 0.25 to 0.1 when sliding velocity increases. Finally this works establishes that a TiN layer deposited on carbide tools is not able to modify friction properties.     

A novel approach to simulate segregation at the centreline of continuously cast steel using laser-scanning confocal microscopy

A concentric solidification technique was employed to simulate the segregation of alloying elements that occur during solidification at the centreline of continuously cast steel. Microstructural development of low carbon steel upon solidification has been observed in situ in a laser-scanning confocal microscope. Sulphide precipitates that formed in the last remaining liquid were identified, and evidence is provided that segregation occurring at the centreline of steel slabs can reasonably be simulated by the use of the concentric solidification technique.     

Application of ion-beam etching techniques to the fine structure of biological specimens as examined with a field emission SEM at low voltage

The term “etching,” in electron microscopy, refers to the removal of specimen surface layers and includes chemical, electrolytic, and ion-beam methods. The ion-beam etching process is used to remove layers of a target material by bombarding it with ionized gas molecules. Recently, the method has been applied to the field of biological specimens; however, the practical procedures for such organic materials have not been developed. In the present study, we used an apparatus in which a beam of argon ions is collimated and focused by electrostatic lenses onto an appropriate target. We demonstrated the optimum conditions to observe biological specimens that were treated with osmium tetroxide and tannic acid. The specimens were examined uncoated at low accelerating voltage using a field emission scanning electron microscope. According to our experiments, when a biological specimen was observed under high-resolution conditions at over 50,000x magnification, the optimum condition of ion-beam etching consisted of an accelerating voltage of E = 1 keV and an ion-beam dose of It = 360 ～ 400 μA. min, depending on parts of the specimens. In order to decrease overetching, we had to choose factors such as E = 1 ～ 2 keV and It = 500 μA. min.