Application of sensitive,high‐resolution imaging at a commercial lab‐based X‐ray micro‐CT system using propagation‐based phase retrieval

Several dedicated commercial lab‐based micro‐computed tomography (μCT) systems exist, which provide high‐resolution images of samples, with the capability to also deliver in‐line phase contrast. X‐ray phase contrast is particularly beneficial when visualizing very small features and weakly absorbing samples. The raw measured projections will include both phase and absorption effects. Extending our previous work that addressed the optimization of experimental conditions at the commercial ZEISS Xradia 500 Versa system, single‐distance phase‐contrast imaging is demonstrated on complex biological and material samples. From data captured at this system, we demonstrate extraction of the phase signal or the correction of the mixed image for the phase shift, and show how this procedure increases the contrast and removes artefacts. These high‐quality images, measured without the use of a synchrotron X‐ray source, demonstrate that highly sensitive, micrometre‐resolution imaging of 3D volumes is widely accessible using commercially advanced laboratory devices.     

In situ TEM studies of micron‐sized all‐solid‐state fluoride ion batteries: Preparation,prospects, and challenges

Trustworthy preparation and contacting of micron‐sized batteries is an essential task to enable reliable in situ TEM studies during electrochemical biasing. Some of the challenges and solutions for the preparation of all‐solid‐state batteries for in situ TEM electrochemical studies are discussed using an optimized focused ion beam (FIB) approach. In particular redeposition, resistivity, porosity of the electrodes/electrolyte and leakage current are addressed. Overcoming these challenges, an all‐solid‐state fluoride ion battery has been prepared as a model system for in situ TEM electrochemical biasing studies and first results on a Bi/La_0.9Ba_0.1F_2.9 half‐cell are presented. Microsc. Res. Tech. 79:615–624, 2016. © 2016 Wiley Periodicals, Inc.     

Establishing the archaeo‐metallurgic ornamentation process of an axe from the bronze age by OM,SEM‐EDX,and Micro‐FTIR

Our article presents the results of the analyses we performed by corroborating the Optical Microscopy, Scanning Electron Microscopy, Energy Dispersive Xray Analysis and micro Fourier Transformed InfraRed Analysis techniques to identify the archaeo‐metallurgic casting and ornamentation procedure of a decorated disk‐butted axe, which was discovered recently east of the Carpathian mountains, in the Moldavian Plateau. There are few known axes of that type found (A1, according to the usual typologies), as they are specific to the Middle Bronze Age period west of the Carpathians—the Wietenberg, Suciu de Sus, and Otomani‐Füzesabony cultures. The experimental data on the item under study revealed the fact that after casting it in molds made from porous silicone‐based stone, the object was coated with a thin layer, by immersing it in a lightly fusible tin alloy, whose main alloy component was copper and arsenic and iron as secondary components. After refining the shiny white layer, they applied a beautiful decoration pattern made by incision and engraving. This battle axe was an indication of higher status, such items usually being owned by community leaders. This important fact proves that the ancient metallurgic craftsmen were able to elaborate and manufacture various alloys from which they made beautiful objects and it also offers a new insight into the social and symbolic function of certain antique bronze items. Microsc. Res. Tech. 77:918–927, 2014. © 2014 Wiley Periodicals, Inc.     

Characterization of Cobalt Oxide and Calcium‐Aluminum Oxide nano‐catalyst through Scanning Electron Microscopy,X‐ray diffraction,and Energy Dispersive X‐ray Spectroscopy

The Cobalt Oxide and Calcium‐Aluminum Oxide nano‐catalysts were analyzed using Scanning Electronic Microscopy (SEM), X‐ray diffraction (XRD), and dispersive X‐ray spectroscopy (EDX) techniques. Preliminary results showed that the particles of Cobalt Oxide exhibit sponge like morphology and homogenous distribution as per confirmation via SEM. Its average particle size ranges to 30.6 nm demonstrating enormous number of pores and aggregative in nature. Its various peaks were ranging from 19.2 to 65.4 after XRD analysis. The highest intensity was observed at 36.9 position. The energy dispersive spectroscopy techniques were used to calculate the elements present in sample according to their weight and atomic percentage. The cobalt oxide contain cobalt as the most abundant element with 46.85 wt% and 18.01 atomic percent. It contain oxygen with 30.51 wt% and 43.19 atomic percent. Whereas, SEM of calcium aluminum oxide showed random morphology. According to the calculation of Scherrer equation regarding XRD analysis, it was distributed homogenously with particle size ranges from 30 to 40 nm. Its porous morphology was due to the interconnecting gaps between different particles. It result the eight peaks ranging from 18.1 to 62.7 in XRD spectrum. The highest intensity observed at 35.1 with average crystallite particle size of 25.6 nm. The calcium aluminum oxide contain aluminum 7.45 wt% and 6.93 atomic percent. The calcium was the most abundant element with54.7 wt% and 34.24 atomic percent followed by oxygen with 37.26 wt% and 58.42 atomic percent. It was concluded that the SEM, XRD, and EDX are the most significant techniques to characterize nano‐catalysts in particular and other compounds generally.     

Applicability of ring‐on‐disc and pin‐on‐plate test methods for Cu–steel and Al–steel systems for large area conformal contacts

This study compares two methods for model scale testing of ferrous/non‐ferrous tribocouples under large area conformal contact condition, the kind existing in engine components such as journal bearings. Results show that the ring‐on‐disc method is better suited to visualise the performance of such tribosystems compared with the pin‐on‐plate method. The former offers greater sensitivity to minor changes in coefficient of friction and contact potential and is able to determine the thermal stability of the tribosystem under given conditions. Post‐test surface characterisation revealed protective phosphorus‐rich tribofilms on the surface of the steel counterparts from both test methods. Copyright © 2012 John Wiley & Sons, Ltd.     

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.     

Involution dependent changes in distribution and localization of bax,survivin, caspase‐3, and calpain‐1 in the rat endometrium

The endometrial layer of the uterus is characterized by continuous cycle of cell growth and apoptosis in response to hormonal changes. Apoptosis is regulated by several apoptotic regulators, but their significance in involuting uterus has not been well understood. For that reason, aim of this study was to investigate possible role of apoptosis‐related proteins (bax and survivin) and enzymes (caspase‐3 and calpain‐1) in the involuting uterus of the rat, using immunohistochemistry. Our results indicated cytoplasmic and nuclear immunostaining for bax, caspase‐3, calpain‐1 and survivin proteins were found in the endometrial epithelium and stromal cells such as fibroblasts, mast cells and macrophages, and blood vessels; however, calpain‐1 immunoreactivity in the endometrial fibroblast was quite weak or absent. Supranuclear punctate bax immunolabelling was also observed in the endometrial fibroblasts and luminal and glandular epithelial cells from days 1st and 3rd following parturition, respectively. Although survivin was localized in the apical cytoplasm underneath the apical membrane of the luminal epithelium on the 1st and 3rd days, it was also localized in the apicolateral membrane and basal cytoplasm on the 10th and 15th days of involution. Immunostainigs demonstrated that expression patterns of all examined proteins varied with structural changes in the luminal epithelium, and number of immunopositive fibroblasts for bax, caspase‐3 and survivin increased with advance of postpartum days and reached a maximum on postpartum days 10 and 15. These results suggest that the process of postpartum involution of endometrium may be regulated by apoptotic and non‐apoptotic activity of bax, caspase‐3, calpain‐1, and survivin. Microsc. Res. Tech. 79:285–297, 2016. © 2016 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.     

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.     

Particle‐induced x‐ray analysis using focused ion beams

In addition to the production of secondary electrons and secondary ions, characteristic x‐ray emission may also result from ion/solid interactions and is the basis for the well‐known analysis technique referred to as particle‐induced x‐ray emission. Characteristic x‐rays may be emitted by either bombardment by MeV protons or heavy ions of a few keV. The advantage to heavy ions is that the x‐ray yield is confined to the region near the surface defined by the collision cascade. An advantage of heavy ion‐induced x‐ray emission over electron‐induced x‐ray emission is that the Bremsstrahlung is potentially orders of magnitude lower. Thus, ion‐induced x‐ray spectra may provide for superior peak‐to‐noise ratios, and there‐fore, offers trace element sensitivity compared with elec‐tron‐induced x‐ray emission. In addition, the near surface ion/solid interactions also allow for the possibility of surface analysis or depth profiling. A Dual Beam instrument was used to collect focused ion beam‐induced x‐ray (FIBIX) spectra. The acquisition of characteristic x‐rays from targets via FIBIX is demonstrated and compared with scanning electron microscopy‐induced x‐ray energy dispersive spectroscopy spectra and is consistent with the theory described above.     

An analysis of axial deflection of double‐decker high‐precision bearings vis‐à‐vis conventional ball bearings

Axial deflection of double‐decker high‐precision bearings (DDHPBs) under the influence of axial loads has been theoretically analyzed and has been compared with conventional angular contact and deep‐groove ball bearings of the same bore and outer diameter. The analysis, in general, indicates that the ratio of the axial deflection of DDHPBs to that of the conventional angular contact and deep‐groove ball bearings under the influence of identical axial loads is less than unity. The analysis also indicates that angular contact ball bearings mounted back to back for taking the axial load from both directions can be replaced by DDHPBs, which have less axial deflection and longer life under identical applied loads than angular contact and deep‐groove ball bearings. The better dynamic response characteristics, energy efficiency, uniform stress distribution, lower indentation and deflection on the elements of DDHPBs indicate that DDHPBs have relatively better performance characteristics, higher fatigue life and may have higher potential in various industrial applications as compared to that of the conventional bearings under identical operating conditions. Copyright © 2006 John Wiley & Sons, Ltd.     

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.     

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.     

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.     

Image signal‐to‐noise ratio estimation using adaptive slope nearest‐neighbourhood model

A new technique based on nearest neighbourhood method is proposed. In this paper, considering the noise as Gaussian additive white noise, new technique single‐image‐based estimator is proposed. The performance of this new technique such as adaptive slope nearest neighbourhood is compared with three of the existing method which are original nearest neighbourhood (simple method), first‐order interpolation method and shape‐preserving piecewise cubic hermite autoregressive moving average. In a few cases involving images with different brightness and edges, this adaptive slope nearest neighbourhood is found to deliver an optimum solution for signal‐to‐noise ratio estimation problems. For different values of noise variance, the adaptive slope nearest neighbourhood has highest accuracy and less percentage estimation error. Being more robust with white noise, the new proposed technique estimator has efficiency that is significantly greater than those of the three methods.     

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.     

Anti‐friction,anti‐wear and load‐carrying characteristics of environment friendly additive formulation

The extreme pressure (EP), anti‐wear and friction‐reducing characteristics of some of the commercial additive formulation and individual components on which these formulations are based have been studied and compared to characteristics of the components synthesised from naturally available non‐traditional vegetable oils and cashew nut shell liquid that have been refined and partially hydrogenated to improve stability. It has been shown that individual components from sulphurised and phosphosulphurised vegetable oils, esters and hydrogenated cardanol (derived from cashews) have better anti‐wear and friction‐reducing characteristics than the sulphurised olefins and alkylaryl phosphorothioates normally used as EP and anti‐wear additives, while the load‐carrying characteristics of a number of the combination of these derivatives are comparable. It has been shown that all these formulations are rapidly biodegradable and non‐toxic in nature as compared to traditional EP, anti‐wear and friction‐reducing additives, which fill in the category of slightly toxic to harmful. It is possible to formulate energy‐efficient EP gear oils that are fully biodegradable and non‐toxic by a combination of vegetable oil‐based additives of sulphurised vegetable oils, phosphosulphurised methyl recinoleate and phosphosulphurised hydrogenated cardanol amine borate, which meet all the performance characteristics of US steel 224 eg 52100, M‐50 AISI 1010 requirements. Copyright © 2007 John Wiley & Sons, Ltd.