The role of substrates on the structural,optical, and morphological properties of zno nanotubes prepared by spray pyrolysis

ZnO films were deposited onto glass, ITO coated glass, and sapphire substrate by spray pyrolysis, and subsequently annealed at the same temperature of 400°C for 3 h. The role of substrate on the properties of ZnO films was investigated. The structural and optical properties of the films were investigated by X‐ray diffractometer (XRD) and photoluminescence (PL) spectrophotometer, respectively. The surface morphology of the nanostructured ZnO film was investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Crystallographic properties revealed that the ZnO films deposited on sapphire and ITO substrates exhibit a strong c‐axis orientation of grains with hexagonal wurtzite structure. Extremely high UV emission intensity was determined in the film on ITO. The different luminescence behaviors was discussed, which would be caused by least value of strain in the film. Films grown on different substrates revealed differences in the morphology. ZnO films on ITO and sapphire substrates revealed better morphology than that of the film on glass. AFM images of the films prepared on ITO show uniform distribution of grains with large surface roughness, suitable for application in dye sensitized solar cells. Microsc. Res. Tech. 77:211–215, 2014. © 2013 Wiley Periodicals, Inc.     

Novel techniques of preparing TEM samples for characterization of irradiation damage

Focus ion beam preparation of transmission electron microscopy (TEM) samples has become increasingly popular due to the relative ease of extraction of TEM foils from specific locations within a larger sample. However the sputtering damage induced by Ga ion bombardment in focus ion beam means that traditional electropolishing may be a preferable method. First, we describe a special electropolishing method for the preparation of irregular TEM samples from ex‐service nuclear reactor components, spring‐shaped spacers. This method has also been used to prepare samples from a nonirradiated component for a TEM in situ heavy ion irradiation study. Because the specimen size is small (0.7 × 0.7 × 3 mm), a sandwich installation is adopted to obtain high quality polishing. Second, we describe some modifications to a conventional TEM cross‐section sample preparation method that employs Ni electroplating. There are limitations to this method when preparing cross‐section samples from either (1) metals which are difficult to activate for electroplating, or (2) a heavy ion irradiated foil with a very shallow damage layer close to the surface, which may be affected by the electroplating process. As a consequence, a novel technique for preparing cross‐section samples was developed and is described.     

单晶蓝宝石的延性研磨加工

为实现单晶蓝宝石的延性研磨加工,采用纳米压痕和划痕法测试并分析了单晶蓝宝石(0001)面的微纳力学特性,建立了单颗圆锥状磨粒的压入模型并计算了延性研磨加工的受力临界条件,分析了金刚石磨粒嵌入合成锡研磨盘表面的效果.对单晶蓝宝石进行了延性研磨加工试验,采用NT9800白光干涉仪、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等方法分析了单晶蓝宝石的延性研磨表面特征.试验结果表明:采用纳米压痕和划痕法可以为单晶蓝宝石的延性研磨加工提供工艺参数,单晶蓝宝石的延性堆积的极限深度为100 nm,金刚石磨粒的嵌入及在适当载荷下可以实现蓝宝石的延性研磨加工,实验条件下的最佳载荷为21 kPa,延性研磨后单晶蓝宝石表面划痕深度的分布情况较好,分散性小,研磨后的表面发生了位错滑移变形.     

Combining Ar ion milling with FIB lift-out techniques to prepare high quality site-specific TEM samples

Focused ion beam (FIB) techniques can prepare site‐specific transmission electron microscopy (TEM) cross‐section samples very quickly but they suffer from beam damage by the high energy Ga⁺ ion beam. An amorphous layer about 20–30 nm thick on each side of the TEM lamella and the supporting carbon film makes FIB‐prepared samples inferior to the traditional Ar⁺ thinned samples for some investigations such as high resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS). We have developed techniques to combine broad argon ion milling with focused ion beam lift‐out methods to prepare high‐quality site‐specific TEM cross‐section samples. Site‐specific TEM cross‐sections were prepared by FIB and lifted out using a Narishige micromanipulator onto a half copper‐grid coated with carbon film. Pt deposition by FIB was used to bond the lamellae to the Cu grid, then the coating carbon film was removed and the sample on the bare Cu grid was polished by the usual broad beam Ar⁺ milling. By doing so, the thickness of the surface amorphous layers is reduced substantially and the sample quality for TEM observation is as good as the traditional Ar⁺ milled samples.     

Effect of sample bending on diffracted intensities observed in CBED patterns of plan view strained samples

Convergent beam electron diffraction is used to study the effect of the sample bending on diffracted intensities as observed in transmission electron microscopy (TEM). Studied samples are made of thin strained semiconductor Ga(1-)(x)In(x)As epitaxial layers grown on a GaAs substrate and observed in plan view. Strong variations of the diffracted intensities are observed depending on the thinning process used for TEM foil preparation. For chemically thinned samples, strong bending of the substrate occurs, inducing modifications of both kinematical and dynamical Bragg lines. For mechanically thinned samples, bending of the substrate is negligible. Kinematical lines are unaffected whereas dynamical lines have slightly asymmetric intensities. We analyse these effects using finite element modelling to calculate the sample strain coupled with dynamical multibeam simulations for calculating the diffracted intensities. Our results correctly reproduce the qualitative features of experimental patterns, clearly demonstrating that inhomogeneous displacement fields along the electron beam within the substrate are responsible for the observed intensity modifications.     

Advantages of embedment‐free section transmission electron microscopy

The usefulness of embedment‐free section transmission electron microscopy (TEM) is stressed for present and future morphological analyses, and several examples are demonstrated which are revealed in sections for the first time by this method: en‐face views of slit diaphragm of renal glomerulus and fenestrated diaphragm of capillary endothelium, transparency of neural myelin, attenuated endothelium and some basement laminae, labyrinth architecture of vacuoles within lipid droplets, and enhanced 3D effect of ultrastructures, the latter of which is the case in electron tomography. In addition, the biological significance of structured appearance (microtrabecular lattices) of the cytoplasmic matrix, which is disclosed by this method, are briefly reviewed in relation to the sol–gel transition of cytoplasmic heterogenous proteins. Since the ultrastructures of various cells and tissues in this method are confirmed to be well correspondent to those in conventional epoxy section TEM except for isotropic dimensional changes, and because there is no necessity for any special expensive equipments other than those for the conventional TEM, the embedment‐free section TEM method with these advantages, deserves much more wide application to the morphological research including electron tomography. Microsc. Res. Tech. 76:1257–1265, 2013. © 2013 Wiley Periodicals, Inc.     

Atomic force microscope (AFM) combined with the ultramicrotome: a novel device for the serial section tomography and AFM/TEM complementary structural analysis of biological and polymer samples

A new device (NTEGRA Tomo) that is based on the integration of the scanning probe microscope (SPM) (NT‐MDT NTEGRA SPM) and the Ultramicrotome (Leica UC6NT) is presented. This integration enables the direct monitoring of a block face surface immediately following each sectioning cycle of ultramicrotome sectioning procedure. Consequently, this device can be applied for a serial section tomography of the wide range of biological and polymer materials. The automation of the sectioning/scanning cycle allows one to acquire up to 10 consecutive sectioned layer images per hour. It also permits to build a 3‐D nanotomography image reconstructed from several tens of layer images within one measurement session. The thickness of the layers can be varied from 20 to 2000 nm, and can be controlled directly by its interference colour in water. Additionally, the NTEGRA Tomo with its nanometer resolution is a valid instrument narrowing and highlighting an area of special interest within volume of the sample. For embedded biological objects the ultimate resolution of SPM mostly depends on the quality of macromolecular preservation of the biomaterial during sample preparation procedure. For most polymer materials it is comparable to transmission electron microscopy (TEM). The NTEGRA Tomo can routinely collect complementary AFM and TEM images. The block face of biological or polymer sample is investigated by AFM, whereas the last ultrathin section is analyzed with TEM after a staining procedure. Using the combination of both of these ultrastructural methods for the analysis of the same particular organelle or polymer constituent leads to a breakthrough in AFM/TEM image interpretation. Finally, new complementary aspects of the object's ultrastructure can be revealed.     

Spine micromorphology of normal and hyperhydric Mammillaria gracilis Pfeiff. (Cactaceae) shoots

Artificial conditions of tissue culture affect growth and physiology of crassulacean acid metabolism plants which often results in formation of hyperhydric shoots. In in vitro conditions Mammillaria gracilis Pfeiff. (Cactaceae) growth switches from organized to unorganized way, producing a habituated organogenic callus which simultaneously regenerates morphologically normal as well as altered hyperhydric shoots. In this study, influence of tissue culture conditions on morphology of cactus spines of normal and hyperhydric shoots was investigated. Spines of pot‐grown Mammillaria plants and of in vitro regenerated shoots were examined with stereo microscope and scanning electron microscope. The pot‐grown plants had 16–17 spines per areole. In vitro grown normal shoots, even though they kept typical shoot morphology, had lower number of spines (11–12) and altered spine morphology. This difference was even more pronounced in spine number (six to seven) and morphology of the hyperhydric shoots. Scanning electron microscopy analysis revealed remarkable differences in micromorphology of spine surface between pot‐grown and in vitro grown shoots. Spines of in vitro grown normal shoots showed numerous long trichomes, which were more elongated on spines of the hyperhydric shoots; the corresponding structures on spine surface of pot‐grown plants were noticed only as small protrusions. Scanning electron microscopy morphometric studies showed that the spines of pot‐grown plants were significantly longer compared to the spines of shoots grown in tissue culture. Moreover, transverse section shape varies from elliptical in pot‐grown plants to circular in normal and hyperhydric shoots grown in vitro. Cluster and correspondence analyses performed on the scanning electron microscope obtained results suggest great variability among spines of pot‐grown plants. Spines of in vitro grown normal and hyperhydric shoots showed low level of morphological variation among themselves despite the significant difference in shoot morphology.     

The fine structure of fenestrated adrenocortical capillaries revealed by in-lens field-emission scanning electron microscopy and scanning transmission electron microscopy

Cell biologists probing the physiologic movement of macromolecules and solutes across the fenestrated microvascular endothelial cell have used electron microscopy to locate the postulated pore within the fenestrae. Prior to the advent of in-lens field-emission high-resolution scanning electron microscopy (HRSEM) and ultrathin m et al coating technology, quick-freeze, platinum-carbon replica and grazing thin-section transmission electron microscopy (TEM) methods provided two-dimensional or indirect imaging methods. Wedge-shaped octagonal channels composed of fibrils interwoven in a central mesh were depicted as the filtering structures of fenestral diaphragms in images of platinum replicas enhanced by photographic augmentation. However, image accuracy was limited to replication of the cell surface. Subsequent to this, HRSEM technology was developed and provided a high-fidelity, three-dimensional topographic image of the fenestral surface directly from a fixed and dried bulk adrenal specimen coated with a 1 nm chromium film. First described from TEM replicas, the “flower-like” structure comprising the fenestral pores was readily visualized by HRSEM. High-resolution images contained particulate ectodomains on the lumenal surface of the endothelial cell membrane. Particles arranged in a rough octagonal shape formed the fenestral rim. Digital acquisition of analog photographic recordings revealed a filamentous meshwork in the diaphragm, thus confirming and extending observations from replica and grazing section TEM preparations. Endothelial cell pockets, first described in murine renal peritubular capillaries, were observed in rhesus and rabbit adrenocortical capillaries. This report features recent observations of fenestral diaphragms and endothelial pockets fitted with multiple diaphragms utilizing a Schottky field-emission electron microscope. In-lens staging of bulk and thin section specimens allowed tandem imaging in HRSEM and scanning TEM modes at 25 kV.     

Transmission Electron Microscopy of Boundary-Lubricated Bearing Surfaces. Part I: Mineral Oil Lubricant

Transmission electron microscopy (TEM) was performed on the near-surface material (depth <500 nm) of tapered roller bearing inner rings (cones) that were tested at two levels of boundary-lubricated conditions in mineral oil with no additives. Site-specific thinning of cross section cone surface sections for TEM analyses was conducted using the focused ion beam (FIB) milling technique. High-resolution structural and compositional characterization of near-surface material and surface layers was performed on an untested cone as well as cones tested at Λ～1.1 and 0.3. This approach revealed near-surface microstructural distortion and grain size gradients that were attributed to surface finishing operations during manufacture. The characteristics of oxide surface layers and micro-cracks on the tested bearing surfaces were evaluated and found to depend on lubrication conditions.     

An electron microscopic analysis on the ultra structural abnormalities in sperm of the common carp Cyprinus carpio L. inhabiting a polluted lake, Umiam (Meghalaya, India)

The present communication reports the ultra structural abnormalities in sperm of a fish species Cyprinus carpio inhabiting a polluted lake, Umiam in North‐East India. Transmission electron microscopy (TEM) revealed absence of differentiation between head and midpiece (neck) of some sperm while scanning electron microscopy (SEM) showed some sperm tails with highly reduced length and some sperm with folded tail. Abnormal shape of some sperm head was also revealed by Scanning electron microscopy. Detachment of membrane from some parts of the sperm head and an outward expansion of the same was observed from Transmission electron micrographs of transverse section of sperm head. The well developed mitochondria surrounding the cytoplasmic channel in the sperm tail, as observed in control were found to be drastically disorganized in fish inhabiting the polluted lake. The study suggests that the fish C. carpio inhabiting the polluted lake Umiam is under severe stress as far as its male reproductive system is concerned. The study further suggests that Electron microscopic approach is extremely important in the assessment of adverse effects of environmental pollution on fish tissue. Microsc. Res. Tech. 2011. © 2011 Wiley Periodicals, Inc.     

Accumulative radial-forward extrusion (ARFE) processing as a novel severe plastic deformation technique

A novel severe plastic deformation (SPD) technique entitled accumulative radial-forward extrusion (ARFE) is introduced for producing ultra-fine grained bulk materials. This method is based on radial-forward extrusion process because of inherent capabilities for imposing extremely high plastic strains on material. ARFE was applied to AA1050 and the ability of this process in significant grain refinement is determined even after single cycle. Transmission electron microscopy (TEM) examination showed ultra-fine grains (UFGs) with the average grain size of 450 nm after one cycle of ARFE. Furthermore, micro-hardness distribution through the part’s section indicates the hardness increase to ～52 Hv from the initial value of ～28 Hv after one cycle of ARFE. In order to further investigate of the accumulated strains, ARFE process was also numerically modelled by finite element method.     

TEM sample preparation by FIB for carbon nanotube interconnects

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.     

Stepped surfaces of sapphire (alpha-Al2O3) with low Miller indices.

Oxygen-annealed surfaces of sapphire with low Miller indices ((0001), [1010], [1120], [1011]) have been studied in both transmission electron microscopy (TEM) and reflection electron microscopy (REM) configurations. The significance of REM diffraction conditions for the determination of the nature of the step heights is discussed. The relationship between the TEM and REM images is explained. The structural features are those that might be expected from considerations of the atom arrangement in the low Miller index planes. The structural features on the surfaces varied with respect to annealing temperature and surface condition. Thermally stable structures that might appear from consideration of the equilibrium-annealing temperature are proposed.     

Microstructural characterization of plasma sprayed Ln2Zr2O7 thermal barrier coatings by electron microscopy methods

The presented article characterized microstructural aspects of thermal barrier coatings (TBCs) analysis using methods of electron microscopy such as electron backscatter diffraction (EBSD), transmission/scanning electron microscopy (S/TEM), and TEM. The analyzed TBC system is based on gadolinium zirconate deposited by air plasma spraying method, and additionally, it was subjected to an oxidation test for 500 hr at a temperature of 1,100°C. Moreover, the morphological characterization of feedstock powder was showed. EBSD analysis revealed the inhomogeneity of feedstock materials in the form of complex phase composition. In the case of deposited coating, this method was used to characterize the crystallite size of zirconate coating and phase composition of thermally grown oxide zone. S/TEM and TEM analysis showed morphological details of this zone but not revealed such phase as perovskite oxide of GdAlO₃ type.     

Microstructural characterization of Ti‐6Al‐4V alloy subjected to the duplex SMAT/plasma nitriding

In this study, microstructural characterization of Ti‐6Al‐4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross‐section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X‐ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X‐ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Microsc. Res. Tech. 76:897–903, 2013. © 2013 Wiley Periodicals, Inc.     

X-ray microanalysis of plants containing the platinum group metals

It has been demonstrated that Water hyacinths, grown hydroponically in a solution containing the platinum group metals, accumulate and concentrate some of these metals in their roots. Root samples were examined in a scanning electron microscope, equipped with an energy dispersive spectrometer (SEM-EDS), and platinum was detected on the surface. Further examination in an electron microprobe analyser (EMPA), using both wavelength dispersive spectrometry (WDS) and EDS, show platinum localized in the epidermal region of the root. Ruthenium was detected in root material taken from plants that had accumulated the complexed metal ion from solution.     

Some failure modes of four clinical bone cements

The fracture or failure behaviours of four commercial acrylic-based bone cements have been examined in tensile, bending and compression modes, and their mechanical properties are reviewed. It was found that Palacos R-40 bone cement had high radiopaque agent concentration, with high surface hardness. It exhibited a much lower bending strength and bending modulus compared with the other three bone cements (CMW1, CMW2000 and Simplex P). The textures of tensile fracture surfaces produced were similar for the four bone cements studied. The fracture surface was fragmented by crevices, which developed through the matrix and around large undissolved polymethylmethacrylate (PMMA) beads. Three bands with different features existed on the bending fracture surfaces, with an abrupt transition between them. It appears that the agglomerates of zirconium dioxide particles are implicated in Palacos R-40 bone cement fracture surface. The examination of compressive failed specimens revealed that a 'yielded crack band' existed across the transverse section. Plastic deformation resulted in the PMMA beads being squashed in the longitudinal direction and dilated in the transverse direction.     

Rapid diagnosis of fungal infection of intravascular catheters in newborns by scanning electron microscopy.

Intravascular catheters carry a significant risk of becoming colonized with bacteria and fungi and are important risk factors of septicemia in premature neonates. The study was undertaken to evaluate whether scanning electron microscopy (SEM) examination of removed catheters can be useful in early diagnosis of plastic infection by Candida, providing information useful for initiation of an eventual therapy. The evolution of biofilms in 28 catheters (umbilical or central) implanted in 24 newborns for prematurity was studied by SEM and transmission electron microscopy (TEM). In 4 of 24 patients, SEM examination revealed the presence of Candida in form of yeast or hyphae. In one of these patients, TEM confirmed the presence of organisms. In each case, hemoculture and culture of the catheter itself confirmed the diagnosis. The study demonstrates that SEM can identify fungi in the biomaterials covering the catheter surface in a few hours, allowing an early diagnosis of plastic infection.     

Atomic force microscopy of histological sections using a new electron beam etching method

In order to examine histological sections of the rat vomeronasal epithelium with the atomic force microscope (AFM), we developed an electron beam etching method that improves the resolution of AFM images. This method results in AFM images comparable to those obtained with the transmission electron microscope (TEM). Ultrathin tissue sections embedded in epoxy resin were observed before and after the treatment with electron beam radiation. Before electron beam treatment, epithelial structures such as the microvilli surface, dendritic processes, the supporting cell layers and the neuronal cell layers were all visible using the AFM. However, only a few subcellular structures could also be resolved. The AFM images were not as clear as those obtained with the TEM. After electron beam treatment, however, the resolution of AFM images was greatly improved. Most of the subcellular structures observed in TEM images, including the inner membrane of mitochondria, ciliary-structure precursor body, junctional complexes between the neurons and supporting cells, and individual microvilli were now visible in the AFM images. The electron beam treatment appeared to melt the embedding resin, bringing subcellular structures into high relief. The result of this study suggests that electron beam etching of histological samples may provide a new method for the study of subcellular structure using the AFM.