Electron beam damage of behenic acid films

The rate of fading of electron diffraction patterns of behenic acid monolayer crystals as well as multilayer crystals was measured at 100 kV at room temperature to investigate the dependence of beam damage on specimen thickness. The diffracted intensities for monolayers and double layers decreased nearly exponentially with electron exposure; however, the intensities for multilayers were unchanged during initial electron exposures, often increased temporarily and then decreased with electron exposure. The critical dose, D_e, defined as the dose at which the diffracted intensity falls to 1/e of its initial value, was 1.0 electrons/Ų for the monolayers, 1.8 electrons/Ų for the double layers and more for multilayers. These results lead to the conclusion that D_e for behenic acid increases nearly linearly with specimen thickness in the range of about 25–100 Å for dose rate of 0.1–2 electrons/Ų min.     

Development and optimization of the production technology of large-size position-sensitive detectors

Results of development and optimization of the production technology of large-size semiconductor position-sensitive X-ray detectors, based on Si(Li)-p-i-n structures and intended for tomographic and environmental problems, are described. The detectors with a 50 × 50 × 2-mm-size sensitive area with 8, 16, and 32 strips were produced. With a voltage of 100–500 V, the energy resolution is 50 and 75–80 keV for electrons with an energy of 1 MeV and for α particles with an energy of 7.65 MeV, respectively, when the dark current is 0.5–1 μA, the capacitance value is 300 pF, and noise is 40 keV.     

On-line recording and processing of CTEM images

The direction dependence of electron energy losses was measured with a Möllenstedt energy analyzer which was attached to a convergent beam electron diffraction camera. High energy losses could be observed by adjusting the potential of the middle electrode. The investigations were performed with perfect MgO single crystal platelets of about 400 Å thickness. K-losses of oxygen and magnesium were analyzed. The greatest effect of the direction dependence was observed for the K-loss of Mg. By these results the validity of the reciprocity theorem was confirmed even for higher energy loss electrons up to at least 1.3 keV for 40 keV primary electrons.     

Influence of the angular distribution of backscattered electrons on signals at different take-off angles in low-voltage scanning electron microscopy (LVSEM)

It is well known that the differential Mott cross section for large-angle elastic scattering shows maxima and minima at angles depending on material and electron energy. For electron energies of 10–30 keV, the averaging by frequent elastic scattering processes results in approximate Lambert angular distributions of backscattered electrons (BSE). However, the present Monte Carlo calculations for electron energies E = 1–5 keV and different angles of incidence show strong deviations from a Lambert distribution which increases with decreasing energy. The signals of the BSE detector with five annular segments for different take-off directions show good agreement with the calculations for normal electron incidence.     

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.     

Temperature-dependent contact phenomena of PVD- and CVD-deposited DLC films sliding on the thin aluminium foil

This paper reports on tribological properties of magnetron-sputtered WC–C and chemical vapour-deposited diamond-like carbon films coated onto hard-metal surfaces when sliding on aluminium foil (0.2 mm nominal thickness) at different temperatures. The study addresses the evolution of the coefficient of friction at the interfaces of the coated hard metal and the aluminium foil under dry-lubrication conditions, in a ball-on-disc configuration. The wear mechanisms of the aluminium foil and the damage produced on the coated surfaces due to the sticking of aluminium were evaluated as a function of the deposited coating and the temperature at their interfaces. Aluminium-transfer to WC–C coated hard-metal surfaces during the sliding operation seemed to be a non-continuous process, which appeared after a certain number of sliding cycles. Temperatures above 70°C accelerated the transfer of aluminium to the WC–C tool surfaces. Chemical vapour-deposited diamond-like carbon films hindered the transfer of aluminium to the hard metal even at temperatures of around 125°C. At greater temperatures, an aluminium–aluminium tribosurface is formed at the interface, which increases the wear rate of the foils and rapidly degrades the quality of coatings of the hard-metal surfaces.     

Electron-specimen interactions in low-voltage scanning electron microscopy

Measurements of the electron range R, and the backscattering coefficient η and the secondary electron yield δ at normal and tilted incidence for different elements show characteristic differences for electron energies in the range of 0.5 to 5 keV, compared with energies larger than 5 keV. The backscattering coefficient does not increase monotonically with increasing atomic number; for example, the secondary electron yield shows a lesser increase with increasing tilt angle. This can be confirmed in back-scattered electron (BSE) and secondary electron (SE) micrographs of test specimens. The results are in rather good agreement with Monte Carlo simulations using elastic Mott cross-sections and a continuous-slowing-down model with a Rao Sahib-Wittry approach for the stopping power at low electron energies. Therefore, this method can be used to calculate quantities of BSE and SE emission, which need a larger experimental effort. Calculations of the angular distribution of BSEs show an increasing intensity with increasing atomic number at high takeoff angles than expected from a cosine law that describes the angular characteristics at high electron energies. When simulating the energy distribution of BSEs, the continuous-slowing-down model should be substituted by using an electron energy-loss spectrum (EELS) that considers plasmon losses and inner-shell ionizations individually (single-scattering-function model). The EELS can be approached via the theory for aluminium or from EELS spectra recorded in a transmission electron microscope for other elements. Measurements of electron range Rα Eⁿ of 1 to 10 keV electrons are obtained from transmission experiments with thin films of known mass thickness. In agreement with other authors the exponent n is lower than at higher electron energies.     

Fixation for biological ultrastructure. II. Cross-linking of bovine serum albumin by nanosecond pulses of ionizing radiation

Very large doses of ionizing radiation were delivered quickly to concentrated albumin solutions by pulses of 500 keV in air. The electrons penetrated the aluminium foil bottom of the test cell and into the solution. A dose of 4.6 Mrad (4.6 × 10⁴ Gy) produced a gel in the albumin solution comparable to the long-term effect of 0.36% glutaraldehyde in the same albumin solution. The cross-links created by the radiation leading to gel formation are probably irreversible and quite different from those leading to gelation in the glutaraldehyde-albumin reaction. Single large pulses of ionizing radiation may be useful for fast fixation of cells and tissues for microscopy.     

Ultraviolet stimulated electron source for use with low energy plasma instrument calibration

We have developed and demonstrated a versatile, compact electron source that can produce a mono-energetic electron beam up to 50 mm in diameter from 0.1 to 30 keV with an energy spread of <10 eV. By illuminating a metal cathode plate with a single near ultraviolet light emitting diode, a spatially uniform electron beam with 15% variation over 1 cm(2) can be generated. A uniform electric field in front of the cathode surface accelerates the electrons into a beam with an angular divergence of <1° at 1 keV. The beam intensity can be controlled from 10 to 10(9) electrons cm(-2) s(-1).     

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.     

The intersecting Kikuchi line technique; critical voltage at any voltage

The close relationship between the critical voltage and the intersecting Kikuchi line technique, two electron diffraction techniques for the accurate determination of structure factor values, is demonstrated by analytical treatment of simple diffraction conditions involving three beams. As an example the value of the 220 structure factor of cubic SiC is determined from convergent-beam electron diffraction using 100 keV electrons.     

Deaccelerating films for picosecond new generation dissectors

This paper describes the selection of deaccelerating films made of aluminum of various thicknesses (300–500 nm) and intended for deacceleration of electrons (with an energy of tens of kiloelectron volts to tens of electron volts) in the developed new generation picosecond dissectors. The designed dissectors should be different by a higher temporal resolution as compared to the maximum reached (~20 ps) in LI-602 dissecting image-tube converters used for diagnosing synchrotron radiation. This paper also presents the results of comparative measurements of emission characteristics of manufactured films in the models of image-tube converters similar in design to a PIF-01/S1 device, which is the basis of the developed dissectors and which provides the maximum temporal resolution of up to 1 ps in the streak mode with the streak speed of ~10¹⁰ cm/s. It is established that, when the energy of the incident electron beam equals 10 to 12 keV, the optimum thickness of the deaccelerating aluminum film is 400 nm with the effective secondary emission coefficient equal to 0.7.     

An interference technique for measuring the thickness of semi-thin and thick sections

An interference method is described for measuring section thickness in the range 0·3–45 μm. An incident illumination objective incorporating a beam splitter and adjustable reference mirror is used to generate interference fringes by reflection from the upper surfaces of sections on glass slides. Sections do not require a reflective coating. The lateral displacement of the zero-order fringe generated using white light is measured in terms of sodium light fringes and photographic enlargement of the fringes allows measurement to ± 30 nm. The method is simple in operation and allows rapid assessment of any local distortions over the entire section area.     

Development of nano-structured Al2O3-TiB2-TiN coatings by combined SHS and laser surface alloying

A powder mixture of aluminium (Al), titania (TiO₂) and hexa-boron nitride (h-BN) was laser-triggered to undergo SHS (self-propagating high temperature synthesis) and was subsequently laser alloyed onto a mild steel substrate surface. A nano-structured coating was formed with high microhardness (～3000 HV_0.05 at the cross-section and ～2600 HV_0.2 on the top surface). X-ray diffraction (XRD) identified the presence of aluminium oxide (Al₂O₃), titanium di-boride (TiB₂), titanium nitride (TiN), iron (Fe) and its borides (FeB, Fe₂B) in the coating. Scanning electron microscopy (SEM) and high resolution transmission electron microscopic (HRTEM) analysis of the coating revealed nano-fibrous titanium-rich reinforcements in a matrix of nano-crystalline alumina. The thickness of titanium di-boride nano-fibres was an order of magnitude higher than the size of nano-alumina crystallites.     

Experimental determination of angular-energy distributions of electrons backscattered by bulk gold and silicon samples

This work describes an experimental study of the backscattering of electron beams with an energy range between 20 and 100 keV. The energy distribution of electrons backscattered by bulk gold and silicon samples at different take-off angles was determined with an original device. The different major sources of noise were studied and then the spectra obtained were processed. Theoretical interpretation of this phenomenon using Monte Carlo simulations will be presented in a future paper.     

An electron diffraction study of paramylon storage granules from Euglena gracilis

Paramylon storage granules from Euglena gracilis were characterized by electron diffraction techniques using electrons of various accelerating voltages: 2 MV for the thick granules and 100 kV for the thinner ones. Intact granules gave well resolved, characteristic (1→3)-β-d glucan fibre diffraction diagrams with the glucan molecular orientation parallel to the longer axis of the granule. Hydrated electron diffraction patterns with better resolution were obtained from thinner granules by examination at low temperatures of quench-frozen specimens. In this case, the pattern indexed on an hexagonal system with a = b= 1·55 + 0·01 nm and c (fibre axis) = 1·86 ± 0·01 nm. Sections of embedded granules provided single crystal-like electron diffraction patterns corresponding to various sections of the reciprocal lattice of (1→3)-β-d glucan (including the hko section). Finally, by scanning electron microscopy, it was shown that the granules swell on contact with water and take up a characteristic ribbed, pumpkin-like shape.     

Measuring the mechanical recoil impulse of a polymeric target upon impact of a high power electron beam

A method for measuring the mechanical recoil impulse of a target produced by the relativistic electron beam of the Calamary accelerator is described. A detector based on a piezoelectric sensor is used in measurements. Results of measurements are presented for the mechanical recoil impulse produced by the relativistic electron beam with an energy as high as 300 keV, a current of up to 30 kA, and a duration of ~100 ns that is incident on an epoxy target. The energy flux density on the target surface is varied in the range of 1–10 GW/cm². The maximum measured impulse value is 0.32 N · s at an energy flux density of 10 GW/cm² (an energy fluence of 810 J/cm2).     

Energy dependence of the relative light output of YAlO<Subscript>3</Subscript>:Ce,Y<Subscript>2</Subscript>SiO<Subscript>5</Subscript>:Ce,and YPO<Subscript>4</Subscript>:Ce scintillators

The nonlinear dependence of the relative light output on the energy deposited in single-crystal scintillation materials YAlO₃:Ce (YAP:Ce), Y₂SiO₅:Ce (YSO:Ce), and YPO₄:Ce (YPO:Ce) has been studied. The investigations have been conducted under quasi-monochromatic X-ray excitation in the energy range of 9.5–100 keV. In addition to the standard technique for measuring the nonproportional scintillator response based on the dependence of the full-energy peak position on the energy of incident radiation, a method is proposed for measuring the light output by X-ray fluorescence peaks. Using this method for YAP:Ce, it is possible to investigate the nonlinear dependence of the light output on the photon energy in the energy range of 2–40 keV. Along with this method, the K-dip spectroscopy method has been proposed and tested by measuring the dependence of the relative light output on the electron energy in the range of 0.1–80.0 keV. The processes resulting in the loss of the scintillation material efficiency at a high ionization density are considered.     

X-ray imaging of various biological samples using a phase-contrast hard X-ray microscope

In this study, we visualized the internal structures of various bio-samples and found the optimum conditions of test samples for the 7 keV hard X-ray microscope of the Pohang light source. From the captured X-ray images, we could observe the intercellular and intracellular structures of dehydrated human cells and mouse tumor tissues without using any staining materials in a spatial resolution better than 100 nm. The metastasized lung tissue, which was several tens of micrometers in thickness, was found to be very well suited to this hard X-ray microscope system, because it is nearly impossible to observe such a nontransparent and thick sample with a high spatial resolution better than 100 nm using any microscopes such as a soft X-ray microscope, an optical microscope, or an electron microscope.     

Fractal behavior of electron trajectories and spatial distributions of secondary electron birth sites in solids

The fractal behavior of electron scattering in solids, simulated by the Monte Carlo method, has been studied. The trajectories of electrons of 1–10 keV primary energies in Si, Cu, Ag, and Au have been simulated. The Hausdorff dimensions of trajectories of primary electrons, trajectories of primary electrons plus secondary electrons, and spatial distributions of secondary electron birth sites have been determined by the box-counting method. The fractal geometry can be used to describe quantitatively the complexity of the electron scattering process in solids.