Time‐lapse lab‐based x‐ray nano‐CT study of corrosion damage

An experimental protocol (workflow) has been developed for time‐lapse x‐ray nanotomography (nano‐CT) imaging of environmentally driven morphological changes to materials. Two case studies are presented. First, the leaching of nanoparticle corrosion inhibitor pigment from a polymer coating was followed over 14 days, while in the second case the corrosion damage to an AA2099 aluminium alloy was imaged over 12 hours. The protocol includes several novel aspects relevant to nano‐CT with the use of a combination of x‐ray absorption and phase contrast data to provide enhanced morphological and composition information, and hence reveal the best information to provide new insights into the changes of different phases over time. For the pigmented polymer coating containing nominally strontium aluminium polyphosphate, the strontium‐rich components within the materials are observed to leach extensively whereas the aluminium‐rich components are more resistant to dissolution. In the case of AA2099 it is found that the initial grain boundary corrosion is driven by the presence of copper‐rich phases and is then followed by the corrosion of grains of specific orientation.     

A tribological study of (2‐sulphurone‐benzothiazole)‐3‐methyl‐dibutyl borate

An organic compound containing S, N, B, and O was synthesised by reacting 2‐mercaptobenzothiazole and formalin in ethanol solution, the resulting product then being reacted with butanol and boric acid in toluene solution. The tribological performance of the novel compound when added to liquid paraffin was evaluated using a four‐ball tester and a ring‐on‐block machine. The relationship between performance and concentration was analysed, and the results show that the compound possesses good antiwear and load‐carrying abilities. The mechanism of action of the additive was investigated using X‐ray photo‐electron spectroscopy (XPS). Surface analysis indicated the formation of a protective film containing FeSO₄, an organo‐sulphur compound, FeS₂, borate, and an organonitrogen compound. This protective film formed during sliding processes contributes to the increase in wear resistance.     

A simple,straightforward correlative live‐cell‐imaging‐structured‐illumination‐microscopy approach for studying organelle dynamics

Most cellular organelles are highly dynamic and continuously undergo membrane fission and fusion to mediate their function. Documenting organelle dynamics under physiological conditions, therefore, requires high temporal resolution of the recording system. Concurrently, these structures are relatively small and determining their substructural organization is often impossible using conventional microscopy. Structured Illumination Microscopy (SIM) is a super resolution technique providing a two‐fold increase in resolution. Importantly, SIM is versatile because it allows the use of any fluorescent dye or protein and, hence, is highly applicable for cell biology. However, similar to other SR techniques, the applicability of SIM to high‐speed live cell imaging is limited. Here we present an easy, straightforward methodology for coupling of high‐speed live cell recordings, using spinning disk (SD) microscopy, with SIM. Using this simple methodology, we are able to track individual mitochondrial membrane fission and fusion events in real time and to determine the network connectivity and substructural organization of the membrane at high resolution. Applying this methodology to other cellular organelles such as, ER, golgi, and cilia will no doubt contribute to our understanding of membrane dynamics in cells. Microsc. Res. Tech. 78:777–783, 2015. © 2015 Wiley Periodicals, Inc.     

Finite‐element heat‐transfer analysis of a PEEK‐steel sliding pair in a pin‐on‐disc configuration

Finite‐element (FE) thermal models have been developed in order to study the temperature distribution in a sliding pair comprising a poly(ether ether ketone) (PEEK) pin and a steel disc in a pin‐on‐disc configuration. First, a moving heat source model for the disc was created. An alternative distributed heat source model was also produced in order to reduce computing time for the evaluation of the moving heat source model by some orders of magnitude. This latter model gave the same results as the moving heat source model, except for a small region just below the moving heat source. On the basis of the distributed heat source approach, a complete axisymmetric FE model for the disc side (taking the effect of thermal resistance between the assembled components into consideration) and a steady‐state quarter model for the pin were developed. Water cooling and air cooling of the steel shaft were also compared. It was found that air cooling allowed a higher temperature in the contact region of the two sliding partners. The experimental results obtained with thermocouples and a thermal camera showed good agreement with the model predictions.     

Real‐space observation of strong metal‐support interaction: state‐of‐the‐art and what's the next

The real‐space resolving of the encapsulated overlayer in the well‐known model and industry catalysts, ascribed to the advent of dedicated transmission electron microscopy, enables us to probe novel nano/micro architecture chemistry for better application, revisiting our understanding of this key issue in heterogeneous catalysis. In this review, we summarize the latest progress of real‐space observation of SMSI in several well‐known systems mainly covered from the metal catalysts (mostly Pt) supported by the TiO₂, CeO₂ and Fe₃O₄. As a comparison with the model catalyst Pt/Fe₃O₄, the industrial catalyst Cu/ZnO is also listed, followed with the suggested ongoing directions in the field.     

Two‐In‐one sample preparation for plan‐VIew TEM

Transmission electron microscopy (TEM) sample preparation requires special skills, it is time consuming and costly, hence, an increase of the efficiency is of primary importance. This article describes a method that duplicates the yield of the conventional mechanical and ion beam preparation of plan‐view TEM samples. As a modification of the usual procedures, instead of one two different samples are comprised in a single specimen. The two pre‐cut slabs, one from each samples, are embedded side by side in the window of a 3 mm dia Ti disk and the specimen is thinned mechanically and by ion milling until perforation that occurs at the interface of the two different slabs. That, with proper implementation, provides acceptable size thin area for the TEM study of both samples. The suitability of the two‐in‐one method has been confirmed through examples. Microsc. Res. Tech. 78:599–602, 2015. © 2015 Wiley Periodicals, Inc.     

Three‐dimensional imaging of whole mouse models: comparing nondestructive X‐ray phase‐contrast micro‐CT with cryotome‐based planar epi‐illumination imaging

In this study, we compare two evolving techniques for obtaining high‐resolution 3D anatomical data of a mouse specimen. On the one hand, we investigate cryotome‐based planar epi‐illumination imaging (cryo‐imaging). On the other hand, we examine X‐ray phase‐contrast micro‐computed tomography (micro‐CT) using synchrotron radiation. Cryo‐imaging is a technique in which an electron multiplying charge coupled camera takes images of a cryo‐frozen specimen during the sectioning process. Subsequent image alignment and virtual stacking result in volumetric data. X‐ray phase‐contrast imaging is based on the minute refraction of X‐rays inside the specimen and features higher soft‐tissue contrast than conventional, attenuation‐based micro‐CT. To explore the potential of both techniques for studying whole mouse disease models, one mouse specimen was imaged using both techniques. Obtained data are compared visually and quantitatively, specifically with regard to the visibility of fine anatomical details. Internal structure of the mouse specimen is visible in great detail with both techniques and the study shows in particular that soft‐tissue contrast is strongly enhanced in the X‐ray phase images compared to the attenuation‐based images. This identifies phase‐contrast micro‐CT as a powerful tool for the study of small animal disease models.     

Diesel‐lubricated ta‐C coatings

Samples coated with tetrahedral amorphous carbon were investigated in two different oscillating test setups regarding their friction and wear properties. As lubricants petrodiesel, rapeseed methyl ester biodiesel and a mixture thereof were used. Compared with a petrodiesel‐lubricated uncoated system, friction was reduced for more than 50% when a tetrahedral amorphous carbon coating was applied and biodiesel added to the lubricant. Impurities of monoglycerides are assumed to be the cause for the friction‐modifying effect. Copyright © 2013 John Wiley & Sons, Ltd.     

Entropy‐assisted image segmentation for nano‐ and micro‐sized networks

Image analysis is an important tool for characterizing nano/micro network structures. To understand the connection, organization and proper alignment of network structures, the knowledge of the segments that represent the materials inside the image is very necessary. Image segmentation is generally carried out using statistical methods. In this study, we developed a simple and reliable masking method that improves the performance of the indicator kriging method by using entropy. This method selectively chooses important pixels in an image (optical or electron microscopy image) depending on the degree of information required to assist the thresholding step. Reasonable threshold values can be obtained by selectively choosing important pixels in a complex network image composed of extremely large numbers of thin and narrow objects. Thus, the overall image segmentation can be improved as the number of disconnected objects in the network is minimized. Moreover, we also proposed a new method for analyzing high‐pixel resolution images on a large scale and optimized the time‐consuming steps such as covariance estimation of low‐pixel resolution image, which is rescaled by performing the affine transformation on high‐pixel resolution images. Herein, image segmentation is executed in the original high‐pixel resolution image. This entropy‐based masking method of low‐pixel resolution significantly decreases the analysis time without sacrificing accuracy.     

Cryo‐scanning x‐ray diffraction microscopy of frozen‐hydrated yeast

We developed cryo‐scanning x‐ray diffraction microscopy, utilizing hard x‐ray ptychography at cryogenic temperature, for the noninvasive, high‐resolution imaging of wet, extended biological samples and report its first frozen‐hydrated imaging. Utilizing phase contrast at hard x‐rays, cryo‐scanning x‐ray diffraction microscopy provides the penetration power suitable for thick samples while retaining sensitivity to minute density changes within unstained samples. It is dose‐efficient and further minimizes radiation damage by keeping the wet samples at cryogenic temperature. We demonstrate these capabilities in two dimensions by imaging unstained frozen‐hydrated budding yeast cells, achieving a spatial resolution of 85 nm with a phase sensitivity of 0.0053 radians. The current work presents the feasibility of cryo‐scanning x‐ray diffraction microscopy for quantitative, high‐resolution imaging of unmodified biological samples extending to tens of micrometres.     

Matrices pattern using FIB; ‘Out‐of‐the‐box’ way of thinking

Focused ion beam (FIB) is an extremely valuable tool in nanopatterning and nanofabrication for potentially high‐resolution patterning, especially when refers to He ion beam microscopy. The work presented here demonstrates an ‘out‐of‐the‐box’ method of writing using FIB, which enables creating very large matrices, up to the beam‐shift limitation, in short times and with high accuracy unachievable by any other writing technique. The new method allows combining different shapes in nanometric dimensions and high resolutions for wide ranges.     

MRT Letter: Two‐photon excitation‐based 2pi Light‐sheet system for nano‐lithography

We propose two‐photon excitation‐based light‐sheet technique for nano‐lithography. The system consists of 2 ‐configured cylindrical lens system with a common geometrical focus. Upon superposition, the phase‐matched counter‐propagating light‐sheets result in the generation of identical and equi spaced nano‐bump pattern. Study shows a feature size of as small as few tens of nanometers with a inter‐bump distance of few hundred nanometers. This technique overcomes some of the limitations of existing nano‐lithography techniques, thereby, may pave the way for mass‐production of nano‐structures. Potential applications can also be found in optical microscopy, plasmonics, and nano‐electronics. Microsc. Res. Tech. 78:1–7, 2015. © 2014 Wiley Periodicals, Inc.     

FE‐SEM observation of swelled seaweed using hydrophilic ionic liquid; 1‐butyl‐3‐methylimidazolium tetrafluoroborate

The method to observe the exact morphology of swelled seaweed as an example of biological material by field emission scanning electron microscopy (FE‐SEM) with the aid of hydrophilic ionic liquid (IL); 1‐butyl‐3‐methylimidazolium tetrafluoroborate is reported. Seaweed was first swelled in 3.5% NaCl solution and then treated with the IL and water mixture in 1:7 weight ratios and centrifuged to remove the excess IL solution. Thus treated seaweed maintained its morphology even at high magnification and did not show drying in the FE‐SEM chamber. This observation technique might be useful for various kinds of biological materials to be observed under FE‐SEM. Microsc. Res. Tech., 2013. © 2012 Wiley Periodicals, Inc.     

Laser‐preparation of geometrically optimised samples for X‐ray nano‐CT

A robust and versatile sample preparation technique for the fabrication of cylindrical pillars for imaging by X‐ray nano‐computed tomography (nano‐CT) is presented. The procedure employs simple, cost‐effective laser micro‐machining coupled with focused‐ion beam (FIB) milling, when required, to yield mechanically robust samples at the micrometre length‐scale to match the field‐of‐view (FOV) for nano‐CT imaging. A variety of energy and geological materials are exhibited as case studies, demonstrating the procedure can be applied to a variety of materials to provide geometrically optimised samples whose size and shape are tailored to the attenuation coefficients of the constituent phases. The procedure can be implemented for the bespoke preparation of pillars for both lab‐ and synchrotron‐based X‐ray nano‐CT investigations of a wide range of samples.     

Chromatographic and non‐chromatographic characterization of poly‐α‐olefins

Both chromatographic and non‐chromatographic techniques were used in the characterization and identification of poly‐α‐olefins. Synthetic base oils, although produced from the same raw material, exhibit different physico‐chemical properties. Their mutual miscibility and behaviour in final engine oils may be predicted from data collected through classical physico‐chemical analysis, simulated distillation chromatography as well as inverse gas chromatography. Copyright © 2007 John Wiley & Sons, Ltd.     

Dimethyl‐2‐[(acridin‐9‐yl)methylidene]‐malonate as fluorescent probe for histochemical analysis

Fluorescent compounds have been widely used for biomolecule labeling in cytochemistry and histochemistry analysis. Here, it is described the optical properties of dimethyl 2‐[(acridin‐9‐yl)methylidene]‐malonate (LPSF/IP‐81), an acridine derivative. This compound was conjugated to Concanavalin A (Con A) lectin and applied as sugar probe in lectin histochemistry. Evaluation of luminescent properties showed that LPSF/IP‐81 is photoluminescent with excitation at 360 nm and emission at 428 nm. Con A hemagglutinating activity and LPSF/IP81 photoluminescence were unaltered after conjugation. Circular dichroism of Con A‐LPSF/IP81 conjugate showed the maintenance of the Con A structure. Lectin histochemistry with Con A‐LPSF/IP81 conjugate demonstrated different pattern recognition studying normal, fibroadenoma, and invasive ductal carcinoma of human breast. These findings indicate that LPSF/IP‐81 can be proposed as an alternative probe for histochemical analysis.     

Herringbone‐grooved bearing with non‐uniform grooves for high‐speed spindle

A hydrodynamic bearing with non‐uniform herringbone grooves has been developed for use with high‐speed motor spindles. The grooves gradually become narrower, shallower and less straight (curved) towards the herringbone centre along axial direction, resulting in an increased pumping effect of the spiral grooves. The optimum dimensions of the grooves for increasing the critical bearing number were clarified theoretically, and bearings with non‐uniform herringbone grooves were found to increase the critical bearing number against the half‐frequency whirl up to about 50% in comparison to bearings with uniform herringbone grooves. Experiments to investigate the suitability of the proposed bearing for high‐speed spindles showed that the maximum rotational speed of a spindle with this bearing was about 20% higher, close to the theoretically predicted 23%, and thus proved that application of this bearing should enable spindles to achieve faster stable rotation as theoretically expected. Copyright © 2010 John Wiley & Sons, Ltd.