In situ observations of unusual dislocation mechanisms in the intermetallic alloy Ti3Al

In situ straining experiments in a transmission electron microscope have been carried out on a Ti₃Al intermetallic alloy, with the aim of determining the microscopic mechanisms controlling glide in prism, basal and pyramidal planes. Five different antiphase boundary energies have been measured and compared with the corresponding densities of incorrect first nearest neighbour atoms. The determination of a tension–compression asymmetry in pyramidal slip, and the detailed analysis of the complex microscopic mechanisms involved illustrate the efficiency of in situ experiments to solve complex problems in plasticity. A comparison between the properties of the different slip systems shows that they are controlled by different microscopic mechanisms, none of them being of covalent origin.     

Transmission electron microscopy with a liquid flow cell

The imaging of microscopic structures at nanometre-scale spatial resolution in a liquid environment is of interest for a wide range of studies. Recently, a liquid flow transmission electron microscopy (TEM) holder equipped with a microfluidic cell has been developed and shown to exhibit flow of nanoparticles through an electron transparent viewing window. Here we demonstrate the application of the flow cell system for both scanning and conventional transmission electron microscopy imaging of immobilized nanoparticles with a resolution of a few nanometres in liquid water of micrometre thickness. The spatial resolution of conventional TEM bright field imaging is shown to be limited by chromatic aberration due to multiple inelastic scattering in the water, and we demonstrate that the liquid in the cell can be displaced by a gas phase that forms under intense electron irradiation. Our data suggest that under appropriate conditions, TEM imaging with a liquid flow cell is a promising method for understanding the in situ behaviour of nanoscale structures in a prescribed and dynamically changing chemical environment.     

Automated jet polishing of transmission electron microscope specimens for in situ straining

A jet-polishing technique has been developed for use in the preparation of microtensile specimens for HVEM examination. The technique requires the use of a pair of Teflon sheet inserts with rectangular openings in a conventional specimen holder. When inserts with optimum opening dimensions are used, specimens having elliptical holes close to the center of the gauge section are produced with large electron-transparent areas at both ends of the long axis. Annealed metal specimens, such as brass or aluminum, prepared by this method are stronger, and can be handled more easily, than those prepared by conventional methods. An advantage of the technique is that reproducible electropolishing conditions and the automatic detection of perforation by a photocell can be used in the normal way.     

Direct observation by in situ transmission electron microscopy of the behaviour of IF‐MoS2 nanoparticles during sliding tests: influence of the crystal structure

Direct observation of the behaviour of individual inorganic fullerenes (IF)‐MoS₂ nanoparticles in a sliding interface is essential for the understanding of the influence of the intrinsic characteristics of the nanoparticles on their lubrication mechanisms, when they are used as additives in lubricant oil. In this work, in situ transmission electron microscopy sliding tests were performed on two different types of MoS₂ nanoparticles synthesised by two different methods. It is shown that the IF‐MoS₂ nanoparticles having perfect structure with a high crystalline order and without defects are able to roll and to slide under the combined effect of pressure and shear stress, whereas the IF‐MoS₂ nanoparticles containing many defects exfoliate immediately in the same conditions to deliver MoS₂ layers covering the mating surfaces. A link between these results, the lubrication mechanisms of the nanoparticles and their tribological properties at the macro‐scale was established, proving that the lubrication mechanisms of fullerenes depend on their intrinsic characteristics. Copyright © 2013 John Wiley & Sons, Ltd.     

In vitro and in situ experimental model for X-ray microanalysis of intestinal epithelium

Intestinal chloride (Cl) transport is disturbed in a number of diseases. X-ray microanalysis can be used to study the distribution of Cl and other ions in intestinal epithelial cells. In this study it was attempted to establish an experimental system that retains the in vivo elemental composition of intestinal epithelial cells. An in vitro system was set up in which a segment of rat intestine was mounted in a bath and perfused with different fluids. The chloride in the bath or in the perfusion fluid could be exchanged for gluconate or bromide to determine the direction of chloride fluxes. An in situ system was set up in which the animal was anesthetized and a segment of the intestine was perfused with different solutions. In the in vitro experiments the concentration of Na and Cl in the epithelial cells increased and that of K decreased. These changes occurred within the first 30 minutes of incubation. Uptake of chloride occurred mainly from the bath, as seen in experiments where bromide was used as a chloride analog. The concentration gradient between bath and tissue determined the extent of chloride uptake. Addition of glucose to the perfusion fluid and bath did not improve the results. In the in situ system, preservation of the intracellular ion composition was better. Acceptable results were obtained with perfusion with Krebs-Ringer's buffer without glucose for 30 minutes. In this case, the elemental content of the cell did not change appreciably during incubation. If glucose was added, the Na concentration increased in comparison to the control, both in crypt and villus cells. It is concluded that the intestinal epithelium is a sensitive system, very prone to disturbance of its homeostasis. However, the in situ system can be used in studies of agonist-induced ion transport.     

Improvements for imaging ceramics sintering in situ in ESEM

Sintering of green samples of alumina produced by ice‐templating was followed in situ in an environmental scanning electron microscope (ESEM) up to temperatures as high as 1375°C. These alumina samples with well‐defined architectures are of great interest in the field of materials science due to their high specific strength (especially in compression), low density and adaptable porosity. For the present study, they also have the advantage to exhibit an important topography, inducing interesting contrast when imaged in an ESEM. Improvements of the imaging conditions in the ESEM were essential to really follow the sintering process involving formation of necks between grains or shift of the centre of grains. This paper describes the improvements made and the results observed on the sintering process of alumina green samples processed by ice‐templating.     

In-situ thickness measurement of porous alumina by atomic force microscopy and the reflectance wavelength measurement from 400-1000 nm

This article presents a novel method to measure the in situ thickness of porous alumina (PA) films. The PA films were prepared in oxalic acid at 30, 40, and 60 V direct current. Based on the atomic force microscope measurements, PA film porosities and refractive indexes measurements were acquired. With the observation of the reflectance spectra of PA films over the wavelength range 400-1000 nm, the nondestructive thickness measurement of the PA films were accurate and were found to be 3.66, 7.76, and 11.38 mum, respectively. Experiments showed that when the applied voltage increased, the pores diameters and interpore distances were enlarged, and the interference pattern was stronger and exhibited a greater number of oscillations over the given wavelength range, which indicated that the PA film's thickness increased. Our results match with the theoretical predictions and analysis quite well.     

X80管线钢焊接接头TEM观察下的断裂行为对比

对X80管线钢焊接接头3个区域的试样在透射电子显微镜（TEM）下进行原位拉伸试验,通过观察各个区域裂纹的萌生与扩展过程,对其微观断裂行为进行了研究和分析。结果表明：母材区中,裂纹萌生扩展主要以多裂纹起裂为主,表现为沿晶扩展的断裂形式,最后造成在切应力作用下的剪切脆性断裂;热影响区内,主裂纹首先在切应力作用下以45°方向起裂,整个扩展过程是主裂纹钝化、位错发射、主裂纹前方无位错区形成、微裂纹形核、主裂纹与微裂纹连接扩展这一多尺度过程不断重复的过程,最后导致准解理穿晶断裂;焊缝区中,从主裂纹分支出多条裂纹,裂纹均以与拉伸轴成45°的方向起裂,表现为沿晶与穿晶混合的断裂模式,最后造成穿晶脆性解理断裂。