An electron microscopy study of the phase Al3Fe

The phase Al₃Fe (monoclinic C2/m, a = 1·549 nm, b = 0·808 nm, c = 1·248 nm, β = 107·8°) has been studied by transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Crystals were obtained from a direct chill-cast ingot of an Al-0·25 wt% Fe-0·13 wt% Si alloy. Extracted crystals were prepared by dissolving the aluminium phase in butanol and filtering off the particles. The extracted Al₃Fe crystals were mainly (100) platelets. The monclinic lattice was confirmed by tilt experiments and the mirror plane was confirmed by convergent beam electron diffraction. Experimental HREM images from the [100] and [110] projection agreed with images calculated by the multislice method. The interpretation of images in terms of a projected crystal structure is discussed. Common defects in Al₃Fe crystals were: twins on (100) and faults on (001). The (001) faults could be described by a displacement 1/2·[100] on a fault plane at z = 0·5 in the unit cell. A model for (001) faults, based on multiple twinning, is proposed.     

PHOEBE,a prototype scanning laser-feedback microscope for imaging biological cells in aqueous media

Based on the principle of laser-feedback interferometry (LFI), a laser-feedback microscope (LFM) has been constructed capable of providing an axial (z) resolution of a target surface topography of ～ 1 nm and a lateral (x, y) resolution of ～ 200 nm when used with a high-numerical-aperture oil-immersion microscope objective. LFI is a form of interferometry in which a laser's intensity is modulated by light re-entering the illuminating laser. Interfering with the light circulating in the laser resonant cavity, this back-reflected light gives information about an object's position and reflectivity. Using a 1-mW He–Ne (λ = 632·8 nm) laser, this microscope (PHOEBE) is capable of obtaining 256 × 256-pixel images over fields from (10 μm × 10 μm) to (120 μm × 120 μm) in ～ 30 s. An electromechanical feedback circuit holds the optical pathlength between the laser output mirror and a point on the scanned object constant; this allows two types of images (surface topography and surface reflectivity) to be obtained simultaneously. For biological cells, imaging can be accomplished using back-reflected light originating from small refractive-index changes (> 0·02) at cell membrane/water interfaces; alternatively, the optical pathlength through the cell interior can be measured point-by-point by growing or placing a cell suspension on a higher-reflecting substrate (glass or a silicon wafer). Advantages of the laser-feedback microscope in comparison to other confocal optical microscopes include: the simplicity of the single-axis interferometric design; the confocal property of the laser-feedback microscope (a virtual pinhole), which is achieved by the requirement that only light that re-enters the laser meeting the stringent frequency, spatial (TEM₀₀), and coherence requirements of the laser cavity resonator mode modulate the laser intensity; and the improved axial resolution, which is based on interferometric measurement of optical amplitude and phase rather than by use of a pinhole as in other types of confocal microscopes.     

A spectroscopic study of some high-temperature superconductors using a low-temperature STM

We used a scanning tunnelling microscope (STM) to measure both the tunnel current, I, and the dynamic conductance, dI/dV, at 4·2 K for a number of high-transition temperature oxide superconductors. Large spatial variations in the tunnelling characteristics are observed. At low tunnel resistances, all samples show evidence of single electron tunnelling and incremental charging. Results on BiSrCaCu₂O_x show the coexistence of charging with Josephson coupling between grains within the sample. Results on both the Bi sample and a single crystal of YBa₂Cu₃O_6·5+x reveal possible energy gap (2A) values of 17 and 20 meV, respectively. A very sharp 5 meV gap, observed in ceramic samples of YBa₂Cu₃O_6·5+x and Y_0·5Al_0·05Ba₂Cu₃O_6·5+x, may indicate the presence of a lower temperature phase in these samples.     

Direct imaging of paracrystalline phospholipid structure in the electron microscope

A long chain amphiphilic molecule—the phospholipid 1,2-dihexadecyl sn glycerophosphoethanolamine—has been crystallized epitaxially so that the interlamellar molecular periodicity is parallel to the substrate and hence normal to the electron beam in the electron microscope. This has permitted the direct resolution of the 55·6 Å lamellae in unstained crystals at room temperature. The lattice images have shown the presence of line dislocations and lenticular cracks in the crystals. Of significance to their biological properties is that the lattice is undulating with a periodicity of 0·1–0·5 μm. This would also account for the difficulties encountered by X-ray and electron diffraction techniques when examining these crystals.     

Quantitative analysis of electrolytes in frozen dried sections

During recent years our group has employed the technique of electron microprobe analysis to determine the electrolyte concentrations in various epithelial tissues. The specimen preparation is characterized by shock-freezing of small tissue pieces in liquid propane/isopentane mixtures at 77 K, cryosectioning of 1 μm thick serial sections at 170 K and subsequent freeze-drying at 190 K and 10^?4 Pa. The analysis of the frozen dried cryosections is performed in a scanning electron microscope which is equipped with an energy dispersive X-ray detector. The measuring conditions selected are 17–20 kV acceleration voltage and 0·1–0·5 nA probe current. For quantification, the cellular X-ray spectra are compared with those of an internal albumin standard layer. The evaluation of the characteristic X-ray intensities is performed using a computer program. Some critical points of this technique will be discussed.     

Studies on insect fibrous proteins: the structural protein of the ootheca in the praying mantis, Sphodromatis centralis Rehn

Histological studies have been made on the left colleterial gland which secretes the α-type structural protein in the ootheca of Sphodromantis centralis. Three distinct types of secretory cell are present in the gland wall, and each has a complex apical ‘end-apparatus’ composed of closely packed canalicules radiating from a central cavity. Structural protein is synthesized in the cytoplasm, passed through the canalicules into the cavity of the end-apparatus, and extruded into the lumen as strongly birefringent, apparently membrane-free globules. At this stage the globules consist of numerous concentric layers of long, parallel fibrils, 0·05–0·1 μm in diameter. In each successive layer the fibril direction is rotated through an angle of about 18° about an axis perpendicular to the layers, in the manner of cholesteric phase systems. When sectioned, the globules reveal a regular ‘lamellated’ structure similar to that apparent in sections of some insect and crustacean cuticles. A three-dimensional model has been constructed to illustrate this phenomenon. During ootheca formation fibrils become transformed into thin ‘crystalline’ ribbons, about 15 μm long, 1–2 μm wide and 200–300 Å thick. Very regular diamond-shaped ribbons may be obtained in vitro by mixing structural protein globules from dissected left glands with optimum concentrations (0·005–·025 m ) of calcium chloride in unbuffered solution. Experiments suggest that calcium ions play an important part in the natural process of ribbon formation.     

Ponceau 2R staining of proteins and periodic acid bleaching of osmicated subcellular structures on semi-thin sections of tissues processed for electron microscopy: a simplified procedure

An aqueous solution (pH 1·5) of 0·5% Ponceau 2R (C.I. 16150) and 2% periodic acid was used at 318 K to stain proteins (brilliant red) and simultaneously to bleach the osmicated non-proteinaceous cell structures on 1–2 μm thick sections of tissues fixed in glutaraldehyde-osmium tetroxide and embedded in epoxy resins. This H₅IO₆ bleaching-Ponceau 2R staining procedure only stains the proteins so that black-and-white films can be used.     

Applications of medium-voltage STEM for the 3-D study of organelles within very thick sections

Scanning transmission electron microscopy at 300 kV enables the visualization of nucleolar silver-stained structures within thick sections (3–8 μm) of Epon-embedded cells at high tilt angles (–50°; + 50°). Thick sections coated with gold particles were used to determine the best conditions for obtaining images with high contrast and good resolution. For a 6-μm-thick section the values of thinning and shrinkage under the beam are 35 to 10%, respectively. At the electron density used in these experiments (100e^—/Å₂/s) it is estimated that these modifications of the section stabilized in less than 10 min. The broadening of the beam through the section was measured and calculations indicated that the subsequent resolution reached 100 nm for objects localized near the lower side of 4-μm-thick sections with a spot-size of 5·6 nm. Comparing the same biological samples, viewed alternately in CTEM and STEM, demonstrated that images obtained in STEM have a better resolution and contrast for sections thicker than 3 μm. Therefore, the visualization of densely stained structures, observed through very thick sections in the STEM mode, will be very useful in the near future for microtomographic reconstruction of cellular organelles.     

The point-spread function of a confocal microscope: its measurement and use in deconvolution of 3-D data

We have measured the point-spread function (PSF) for an MRC-500 confocal scanning laser microscope using subresolution fluorescent beads. PSFs were measured for two lenses of high numerical aperture—the Zeiss plan-neofluar 63 × water immersion and Leitz plan-apo 63 × oil immersion—at three different sizes of the confocal detector aperture. The measured PSFs are fairly symmetrical, both radially and axially. In particular there is considerably less axial asymmetry than has been demonstrated in measurements of conventional (non-confocal) PSFs. Measurements of the peak width at half-maximum peak height for the minimum detector aperture gave approximately 0·23 and 0·8 μm for the radial and axial resolution respectively (4·6 and 15·9 in dimensionless optical units). This increased to 0·38 and 1·5 μm (7·5 and 29·8 in dimensionless units) for the largest detector aperture examined. The resulting optical transfer functions (OTFs) were used in an iterative, constrained deconvolution procedure to process three-dimensional confocal data sets from a biological specimen—pea root cells labelled in situ with a fluorescent probe to ribosomal genes. The deconvolution significantly improved the clarity and contrast of the data. Furthermore, the loss in resolution produced by increasing the size of the detector aperture could be restored by the deconvolution procedure. Therefore for many biological specimens which are only weakly fluorescent it may be preferable to open the detector aperture to increase the strength of the detected signal, and thus the signal-to-noise ratio, and then to restore the resolution by deconvolution.     

SEM analyses of cathodoluminescence in MgO,CdS and GaAs/GaxAl1–xAs crystals

The method of analysis developed for the study of cathodoluminescence in the scanning electron microscope is briefly outlined. Current studies of cathodoluminescence in three types of crystal are presented. These are: (1) deformed and annealed MgO, (2) CdS into which Ga has been diffused, and (3) double heterostructure GaAs/Ga_xAl_1–xAs laser material.     

Electron Microscope Studies Of Vpe Gainas Layer Structures Suitable For Use As Infrared Leds

Electron microscope investigations have been carried out on vapour grown (100) GaAs/GaInAs structures designed for use as infrared emitters of wavelength 1·06 μm. The structures consist of a GaAs substrate, a graded layer in which the indium concentration is increased from zero to 17 atomic %, and a constant composition Ga_0·83In_0·17As layer which contains a p-n junction. X-ray microprobe analysis of cross-sections of the slices established the uniformity of the grading. TEM analysis showed a dense and extensive asymmetric network of misfit dislocations (1 × 10¹² m^?2 (10⁸ cm^?2)) in the graded layer, threading dislocations and other anomalous contrast features extending from the graded layer through the p-n junction to the surface (local densities of 1 × 10¹¹–1 × 10¹² m^?2 (10⁷–10⁸ cm^?2)), and a planar network of dislocations just below the surface (spacing 0·2–2 μm). SEM EBIC and CL studies of the layer above the junction revealed dark spots, and a cross-grid of dark lines, which could be correlated with the threading defects, and the dislocation network just below the surface, respectively. The SEM results showed that these defects had a deleterious effect on the luminescent and electrical properties of the material in the vicinity of the p-n junction, and would therefore impair the performance of devices made from these layer structures.     

Scanning probe microscopy of biological samples and other surfaces

Scanning probe microscopes derived from the scanning tunnelling microscope (STM) offer new ways to examine surfaces of biological samples and technologically important materials. The surfaces of conductive and semiconductive samples can readily be imaged with the STM. Unfortunately, most surfaces are not conductive. Three alternative approaches were used in our laboratory to image such surfaces. 1. Crystals of an amino acid were imaged with the atomic force microscope (AFM) to molecular resolution with a force of order 10^?8 N. However, it appears that for most biological systems to be imaged, the atomic force microscope should be able to operate at forces at least one and perhaps several orders of magnitude smaller. The substitution of optical detection of the cantilever bending for the measurement by electron tunnelling improved the reliability of the instrument considerably. 2. Conductive replicas of non-conductive surfaces enabled the imaging of biological surfaces with an STM with a lateral resolution comparable to that of the transmission electron microscope. Unlike the transmission electron microscope, the STM also measures the heights of the features. 3. The scanning ion conductance microscope scans a micropipette with an opening diameter of 0·04-0·1 μm at constant ionic conductance over a surface covered with a conducting solution (e.g., the surface of plant leaves in saline solution).     

Surface structures of YBa2Cu3O7-x,BiCa1·7Sr0·7Cu2Ox and TlCaBaCuO4·5±x investigated by scanning tunnelling microscopy

Surface structures of the high-T_c superconductors YBa₂Cu₃O_7-x, BiCa_1·7Sr_0·7Cu₂O_x and TlCaBaCuO_4·5±x have been investigated with scanning tunnelling microscopy. The observed features include well-organized stripe corrugations in Y-Ba-Cu-O as well as orientated flake-like structures and steps with various heights in the Bi- and Tl-compounds. These observations suggest strong local variations of the elastic and electronic properties of the investigated materials.     

Corrosion and wear behaviour of ZrN thin films

Abstract

ZrN coating is an alternative candidate to replace the conventional TiN coating especially for high temperature oxidation resistance applications. ZrN coatings of varying thickness (1·5, 2·0, 2·5, 3·0 and 4·0 μm) were deposited on 316 stainless steel substrates by cathodic arc evaporation in a reactive nitrogen atmosphere. The influences of lamellae thickness on the microstructure, tribological and corrosive properties of the films were investigated. The coefficient of steady state friction of the films ranged from 0·213 to 0·659. The corrosion resistance of the coatings was tested in 1 N H₂SO₄ solution. The results indicate that the microstructure, wear and corrosion properties of the films were dependent on lamellae thicknesses and film structure.     

Confocal microscopy in the analysis of the etched nuclear particle tracks in polymers

The possibility of the morphometric analysis of etched tracks, induced by protons and alpha particles in the organic polymer allyl diglycol carbonate (CR-39), using the confocal scanning laser microscope (CSLM), was studied. The detectors were investigated in two groups of irradiation experiments, namely: (a) irradiated with mono-energetic neutrons of energy 1–2 MeV, (b) exposed to the alpha radiation from ²²²Rn and its progeny. Both groups were irradiated at normal incidence. Radiation-induced latent tracks were electrochemically etched, and their morphometric parameters were investigated in the reflection mode by using the 488-nm spectral line of an argon ion laser. A constant number of up to 200 optical sections in Z-scan mode was taken through each selected etched track at vertical spacings of 0·642 μm. Successive reconstructions of Z-sections were used to determine the following parameters: the mean radius of the opening channel, the maximum diameter and the length of the track, and the angle of the track wall to the surface of the sample. The results show that tracks produced by alpha particles differ from those induced by protons. The radius of the opening channel of alpha-particle-induced tracks ranges from 7·9 to 11 μm, whereas for protons the same parameter ranges between 2·0 and 3·8 μm for a specific electrochemical etch procedure.     

Automated Microscope-Absorption-Spectrophotometry Of Rock-Forming Minerals In The Range 40,000–5000 Cm−1 (250–2000 Nm)

To measure polarized absorption spectra of microcrystals of 3dⁿ-ion bearing silicate minerals, computer processed, microscope-spectrophotometric methods have been developed. Absorbance, log (I₀/I), can be measured with high relative accuracy (near u.v. and vis: ±0·002 to 0·001; n.i.r.: ±0·004 to 0·002), and relatively small spectral band widths are available. Hence, weak spin-forbidden dd-bands of 3dⁿ-ions can be recognized alongside spin-allowed dd-transitions without artificial broadening of absorption bands due to finite resolution. The smallest area from which absorption spectra can be taken is 8 μm in diameter. As one example of the many applications in mineralogy and material sciences, absorption spectra of a natural spessartine garnet, Spess_69·7Alm_30·0Gross_0·05, containing Mn²⁺, Fe²⁺, and traces of Fe³⁺ as 3dⁿ-ions, and of a pure Mn²⁺-garnet, Spess₆₇Gross₃₃, are presented. From these it is evident that bands in natural spessartines at ～ 26,900, 23,200 cm^?1 which were assigned to dd-transitions in Fe³⁺⁽⁶⁾, have to be reassigned to Mn²⁺⁽⁸⁾. Comparison of spectra obtained with the microscopic equipment described with those obtained by means of conventional macroscopic equipment prove that the methods described produce true spectra.     

Structure and morphology of Mg–Al–Fe‐mixed oxides derivedfrom layered double hydroxides

The influences of the nature and the extent of M(III) ion substitution on the structure, morphology and surface properties of layered double hydroxides, LDHs [Mg_1?x M(III)_x(OH)₂](CO₃)_x/n·mH₂O, M(III) being Al or/and Fe and x= M(III)/[(Mg+M(III)], and derived mixed oxides were investigated. Three series: Mg?Al, Mg?Al?Fe and Mg?Fe were synthesized using low supersaturation co‐precipitation method at constant pH, with different Mg : Al : Fe ratio and x in the wide range from 0.15 to 0.7 in order to obtain complex, multi‐phase systems with disordered structure, developed surface area, acid–base and redox properties favourable for catalytic application. The morphology of LDHs and their derived mixed oxides did not change considerably although pronounced changes in structural and surface properties occur by thermal decomposition. The increase in Al amount, as well as the deviation of M(III) content from the optimal range for the single LDH phase synthesis, causes the formation of smaller particles and decrease of mixed oxide crystallite size. The nature and amount of M(III) influence the development of surface area, after thermal treatment, depending mainly on the presence of smaller mesopores, not visible by scanning electron microscope. Although the particle size has no considerable influence on the value of the surface area, it was observed that the samples with smaller particles (Mg–Al and Mg–Al–Fe series) have also higher surface area compared with the samples with larger particles (Mg–Fe series).     

Structure characterization of pulsed laser deposited MoS x –WSe y composite films of tribological interests

Pulsed laser deposition (PLD) was employed to grow MoS _x –WSe _y composite films, where x = 1.18, y = 0.78. Scanning electron micrographs show that the films have a dense granular morphology. Crystallization, d-spacing and hexagonal sheet curvature within the film were studied with X-ray diffraction, electron diffraction and transmission electron microscopy. A predominant hexagonal MoS _x phase was formed but contained W and Se, which were most likely present as substituents for Mo and S. There was no evidence for two separate crystalline phases. MoS _x –WSe _y composite films exhibited a larger expansion along the c-axis (d-spacing between basal planes) than PLD MoS₂ and WSe₂ films grown by laser ablation of pure targets. The lattice spacing along the a-axis was expanded in comparison to the MoS₂ film, and compressed in comparison to the WSe₂ film. X-ray photoelectron spectroscopy showed a significant sulfur deficiency, and verified both of S and Se bonding in the film. High-resolution electron microscope images exhibited significant curvatures of the (002) basal planes in the films. The bending behavior of basal planes was explained by S vacancies and Se substitution on the atomic site of S layers. The tribological properties of the composite films were measured in dry and wet conditions using a ball-on-disc tribometer. The reduced friction was correlated with the increased crystallinity and increased separation of basal planes in the composite films.     

Thermal detectors of uncooled multi-element infrared imaging Arrays. II. New thermally uninsulated elements

A new approach to constructing the thermal element of a multi-element array on the basis of thin pyroelectric films is developed: the element is neither thermally insulated from the substrate nor separated by a gap from the substrate surface; instead, it operates owing to accumulation of the charge generated by infrared radiation during the frame. A new principle of high-speed modulation of radiation is described. Experimental results for the behavior of the pyroelectric coefficient in barium–strontium niobate films (Ba_xSr_1?xNb₂O₆), whose values reach up to (1–2)·10^?3 C/m², are presented. It is demonstrated that the specific detectivity of sensitive elements 12 × 12 μm in size in the charge accumulation mode is greater than 10⁹ cm · Hz^0.5 ·W^?1.     

Terahertz detectors based on Pb1−x Sn x Te:In films

Results of experimental studies of Pb_1?x Sn _x Te:In films grown by molecular beam epitaxy with the tin concentration close to band inversion are presented. An optimal concentration of indium is determined, and films with x > 0.3 are obtained, where the so-called metal-insulator transition is observed. Photoconductor prototypes are fabricated, and the photocurrent induced by free electron laser radiation in the range of 140–205 µm is measured. A possibility of using photoconductors for recording the own radiation of a body heated to a temperature of 300 K in a passive mode, including systems of image registration in the terahertz spectral range, is estimated.