Quantitative analysis of sputtering due to ion beam bombardment of solids and biological specimens in high resolution electron microscopy

When a positively charged ion beam is used to bombard a solid target, most of the atoms are displaced and sputtered according to the atomic sputtering theory. In the case of biological specimens, most of the bond-breaking molecules in proteins are removed, when based on the molecular sputtering theory. It was found that the thinning rate for solids and the etching rate for biological specimens, when prepared by a normal double fixation and staining method, can be measured from the sputtering yield and density of the specimens. It was also found that the thinning and etching rates depend on the removal weight per sublimation energy and bonding energy, respectively. The angular distribution of sputtering yield, its dependence on incident angle and the secondary electron emission yield were measured, and the optimum etching condition of the incidence was obtained. Experiments showed that the in situ observation of intracellular structures of biological specimens prepared by ion beam etching can be a very effective method in electron microscopy.     

Development of a self-consistent model of dust grain charging at elevated pressures using the method of moments

A model of dust grain charging is constructed using the method of moments. The dust grain charging process in a weakly ionized helium plasma produced by a 100-keV electron beam at atmospheric pressure is studied theoretically. In simulations, the beam current density was varied from 1 to 10⁶ μA/cm². It is shown that, in a He plasma, dust grains of radius 5 μm and larger perturb the electron temperature only slightly, although the reduced electric field near the grain reaches 8 Td, the beam current density being 10⁶ μA/cm². It is found that, at distances from the grain that are up to several tens or hundreds of times larger than its radius, the electron and ion densities are lower than their equilibrium values. Conditions are determined under which the charging process may be described by a model with constant electron transport coefficients. The dust grain charge is shown to be weakly affected by secondary electron emission. In a beam-produced helium plasma, the dust grain potential calculated in the drift-diffusion model is shown to be close to that calculated in the orbit motion limited model. It is found that, in the vicinity of a body perturbing the plasma, there may be no quasineutral plasma presheath with an ambipolar diffusion of charged particles. The conditions for the onset of this presheath in a beam-produced plasma are determined. __________ Translated from Fizika Plazmy, Vol. 29, No. 3, 2003, pp. 214–226. Original Russian Text Copyright ? 2003 by Filippov, Dyatko, Pal’, Starostin.     

Role of secondary electrons and metastable atoms in the electron-beam activation of argon-silane mixtures

The energy and spatial degradation of the primary beam electrons and the production of high-energy secondary electrons in ionizing collisions are analyzed by solving the Boltzmann integral equation for the electron distribution function. The effect of the primary and secondary electrons on the direct ionization of an Ar-SiH₄ mixture, the production of metastable argon atoms, and the dissociation of monosilane molecules is investigated over a wide range of the beam electron energies, argon pressures, and monosilane concentrations. The influence of metastable Ar* atoms on the dissociation of SiH₄ is studied by using the balance equation for metastable argon atoms and the equation for the ambipolar diffusion of ions and low-energy secondary (plasma) electrons in the beam plasma. It is shown that the main contribution to the activation of an Ar-SiH₄ mixture in an electron-beam plasma is provided by secondary electrons with energies higher than the excitation threshold for argon and the dissociation threshold for monosilane, whereas the contribution from metastable argon atoms, though potentially being comparable with that from secondary electrons, is less than in gas-discharge plasmas.     

Charging of submicron structures during silicon dioxide etching in one- and two-frequency gas discharges

A model that combines the Monte Carlo method for calculating electron and ion trajectories in three-dimensional geometry and an analytic approach developed for calculating an electric field in two-dimensional geometry is used to simulate the charging of the surface of periodic submicron SiO₂ structures by electron and ion fluxes in the plasma of a one- and a two-frequency capacitive RF discharge. The energy distribution function of the electrons and ions that come to the bottom of a submicron structure in an argon and an argon-containing plasma is calculated for structures with a width of 11–45 nm and an aspect ratio of d/w = 1–10 (where d and w are the depth and width of the structure). It is shown that secondary electronelectron emission plays an important role in the redistribution of the electric charge and, accordingly, of the electric potential in a submicron structure. It is demonstrated that, when the secondary electron-electron emission mechanism is taken into account, the ion energy spectrum at the bottom of a submicron structure is shifted toward lower energies and becomes broader in comparison with the spectrum of an ion flux from an RF discharge plasma. Moreover, the shift and broadening depend only on the secondary electron-electron emission coefficient, the energy of the charged particles, and the aspect ratio.     

Focused ion beam (FIB)/scanning electron microscopy (SEM) in tissue structural research

The focused ion beam (FIB) and scanning electron microscope (SEM) are commonly used in material sciences for imaging and analysis of materials. Over the last decade, the combined FIB/SEM system has proven to be also applicable in the life sciences. We have examined the potential of the focused ion beam/scanning electron microscope system for the investigation of biological tissues of the model organism Porcellio scaber (Crustacea: Isopoda). Tissue from digestive glands was prepared as for conventional SEM or as for transmission electron microscopy (TEM). The samples were transferred into FIB/SEM for FIB milling and an imaging operation. FIB-milled regions were secondary electron imaged, back-scattered electron imaged, or energy dispersive X-ray (EDX) analyzed. Our results demonstrated that FIB/SEM enables simultaneous investigation of sample gross morphology, cell surface characteristics, and subsurface structures. The same FIB-exposed regions were analyzed by EDX to provide basic compositional data. When samples were prepared as for TEM, the information obtained with FIB/SEM is comparable, though at limited magnification, to that obtained from TEM. A combination of imaging, micro-manipulation, and compositional analysis appears of particular interest in the investigation of epithelial tissues, which are subjected to various endogenous and exogenous conditions affecting their structure and function. The FIB/SEM is a promising tool for an overall examination of epithelial tissue under normal, stressed, or pathological conditions.     

Experimental study of the dynamics of neutron emission from the GOL-3 multimirror trap

In experiments on the plasma heating and confinement in the GOL-3 multimirror trap, a deuterium plasma with a density of ～10¹⁵ cm^?3 and an ion temperature of 1–2 keV is confined for more than 1 ms. The plasma is heated by a relativistic electron beam. The ion temperature, which was measured by independent methods, reached 1.5–2 keV after the beginning of the beam injection. Since such a fast ion heating cannot be explained by the classical energy transfer from electrons to ions through binary collisions, a theoretical model of collective energy transfer was proposed. In order to verify this model, a new diagnostics was designed to study the dynamics of neutron emission from an individual mirror cell of the multimirror trap during electron beam injection. Intense neutron bursts predicted by this model were detected experimentally. Periodic neutron flux modulation caused by the macroscopic plasma flow along the solenoid was observed. The revealed mechanism of fast ion heating can be used to achieve fusion temperatures in the multimirror trap.     

Variable chlorophyll a fluorescence from P-700 enriched Photosystem I particles dependent on the redox state of the reaction centre

1. Photosystem I particles enriched in P-700 prepared by Triton X-100 treatment of chloroplasts show a light-induced increase in fluorescence yield of more than 100% in the presence of dithionite but not in its absence.2. Steady state light maintains the P-700, of these particles, in the oxidised state when ascorbate is present but in the presence of dithionite only a transient oxidation occurs.3. EPR data show that, in these particles, the primary electron acceptor (X) is maintained in the reduced state by light at room temperature only when the dithionite is also present. In contrast, the secondary electron acceptors are reduced in the dark by dithionite.4. Fluorescence emission and excitation spectra and fluorescence lifetime measurements for the constant and variable fluorescence indicate a heterogeneity of the chlorophyll in these particles.5. It is concluded that the variable fluorescence comes from those chlorophylls which can transfer their energy to the reaction centre and that the states PX and P⁺X are more effective quenchers of chlorophyll fluorescence than PX^?, where P is P-700.     

2.5-Dimensional numerical simulation of a high-current ion linear induction accelerator

Results are presented from numerical particle simulations of the transport and acceleration of a high-current tubular ion beam through one to five magnetically insulated accelerating gaps. The ion beam is neutralized by an accompanying electron beam. The possibility of transporting a high-current neutralized ion beam through five cusps is demonstrated. It is shown that the quality of the distribution function of a high-current ion beam at the exit from the accelerator can be substantially improved by optimizing the energy of the neutralizing electron beam. It is also shown that, by injecting additional high-current electron beams into the cusps, the accelerated ion beam can be made more monoenergetic and its divergence can be reduced.     

Monte Carlo transport of swift protons and light ions in water: The influence of excitation cross sections,relativistic effects,and Auger electron emission in w-values

PurposeTo develop a particle transport code to compute w-values and stopping power of swift ions in liquid water and gases of interest for reference dosimetry in hadrontherapy. To analyze the relevance of inelastic and post-collisional processes considered.MethodsThe Monte Carlo code MDM was extended to the case of swift ion impact on liquid water (MDM-Ion). Relativistic corrections in the inelastic cross sections and the post-collisional Auger emission were considered. The effects of introducing different electronic excitation cross sections were also studied.ResultsThe stopping power of swift ions on liquid water, calculated with MDM-Ion, are in excellent agreement with recommended data. The w-values show a strong dependence on the electronic excitation cross sections and on the Auger electron emission. Comparisons with other Monte Carlo codes show the relevance of both the processes considered and of the cross sections employed. W and w-values for swift electron, proton, and carbon ions calculated with the MDM and MDM-Ion codes are in very close agreement with each other and with the 20.8 eV experimental value.ConclusionWe found that w-values in liquid water are independent of ion charge and energy, as assumed in reference dosimetry for hadrontherapy from sparse experimental results for electron and ion impact on gases. Excitation cross sections and Auger emission included in Monte Carlo codes are critical in w-values calculations. The computation of this physical parameter should be used as a benchmark for micro-dosimetry investigations, to assess the reliability of the cross sections employed.     

Electron and proton transfer in the M. smegmatis III2IV2 supercomplex

The M. smegmatis respiratory III₂IV₂ supercomplex consists of a complex III (CIII) dimer flanked on each side by a complex IV (CIV) monomer, electronically connected by a di-heme cyt. cc subunit of CIII. The supercomplex displays a quinol oxidation?oxygen reduction activity of ~90 e^?/s. In the current work we have investigated the kinetics of electron and proton transfer upon reaction of the reduced supercomplex with molecular oxygen. The data show that, as with canonical CIV, oxidation of reduced CIV at pH 7 occurs in three resolved components with time constants ~30 μs, 100 μs and 4 ms, associated with the formation of the so-called peroxy (P), ferryl (F) and oxidized (O) intermediates, respectively. Electron transfer from cyt. cc to the primary electron acceptor of CIV, Cu_A, displays a time constant of ≤100 μs, while re-reduction of cyt. cc by heme b occurs with a time constant of ~4 ms. In contrast to canonical CIV, neither the P → F nor the F → O reactions are pH dependent, but the P → F reaction displays a H/D kinetic isotope effect of ~3. Proton uptake through the D pathway in CIV displays a single time constant of ~4 ms, i.e. a factor of ~40 slower than with canonical CIV. The slowed proton uptake kinetics and absence of pH dependence are attributed to binding of a loop from the QcrB subunit of CIII at the D proton pathway of CIV. Hence, the data suggest that function of CIV is modulated by way of supramolecular interactions with CIII.     

Investigation of the electron energy distribution function in hollow-cathode glow discharges in nitrogen and oxygen

The mechanism for the formation of the inverse electron distribution function is proposed and realized experimentally in a nitrogen plasma of a hollow-cathode glow discharge. It is shown theoretically and experimentally that, for a broad range of the parameters of an N₂ discharge, it is possible to form a significant dip in the profile of the electron distribution function in the energy range ε=2–4 eV and, accordingly, to produce the inverse distribution with df(ε)/d?>0. The formation of a dip is associated with both the vibrational excitation of N₂ molecules and the characteristic features of a hollow-cathode glow discharge. In such a discharge, the applied voltage drops preferentially across a narrow cathode sheath. In the main discharge region, the electric field E is weak (E<0.1 V/cm at a pressure of about p～0.1 torr) and does not heat the discharge plasma. The gas is ionized and the ionization-produced electrons are heated by a beam of fast electrons (with an energy of about 400 eV) emitted from the cathode. A high-energy electron beam plays an important role in the formation of a dip in the profile of the electron distribution function in the energy range in which the cross section for the vibrational excitation of nitrogen molecules is maximum. A plasma with an inverted electron distribution function can be used to create a population inversion in which more impurity molecules and atoms will exist in electronically excited states.     

Space-charge lens for focusing negative ion beams by means of an additional electron ionizer

A space-charge lens created at the Institute of Physics, National Academy of Sciences of Ukraine, to focus negative ion beams using an additional electron ionizer is investigated. In the previous version of the lens, in which the gas was ionized by the ion beam itself, the focal power was quite high (the focal length was ? ≤ 20 cm) but the gas pressure was too great (P ～ 10^?3 torr), which resulted in significant charge-exchange losses of the beam ions. The experimental and theoretical study reported here shows that the use of a 100-eV electron beam as an auxiliary ionizer allows the working pressure in the lens to be significantly reduced. As a result, a simple, inexpensive, and efficient lens has been developed that can be used in systems for transportation of negative ion beams.     

Monte Carlo simulation of single-cell irradiation by an electron microbeam

A model is presented for irradiation of a cellular monolayer by an electron microbeam. Results are presented for two possible window designs, cells plated on the vacuum-isolation window and cells plated on Mylar above the vacuum-isolation window. Even for the thicker dual-membrane window that facilitates tissue culture and allows the target cell to be centered relative to the electron beam, the majority of the calculated beam spreading was contained in a volume typical of the mammalian HeLa cell line. None of the 10⁴ electrons simulated at 25 keV were scattered into the spatial region occupied by neighbors of the target cell. Dose leakage was largest at 50 keV where the mean energy deposited in all neighbors was 21% of that deposited in the target cell. This ratio was reduced to 5% at 90 keV, the highest beam energy simulated. Lineal energy spectra of energy deposition events scored in the nucleus of the target cell became progressively more like the gamma-ray spectrum as the electron beam energy increased. Hence, our simulations provide strong support for the feasibility of a low-LET, single-cell irradiator. Received: 16 March 2000 / Accepted: 9 May 2000     

Efficient isolation of ion beam-induced mutants for homoeologous loci in common wheat and comparison of the contributions of Glu-1 loci to gluten functionality

Key message

Ion beam mutations can be efficiently isolated and deployed for functional comparison of homoeologous loci in polyploid plants, and Glu - 1 loci differ substantially in their contribution to wheat gluten functionality.

Abstract

To efficiently conduct genetic analysis, it is beneficial to have multiple types of mutants for the genes under investigation. Here, we demonstrate that ion beam-induced deletion mutants can be efficiently isolated for comparing the function of homoeologous loci of common wheat (Triticum aestivum). Through fragment analysis of PCR products from M₂ plants, ion beam mutants lacking homoeologous Glu-A1, Glu-B1 or Glu-D1 loci, which encode high molecular weight glutenin subunits (HMW-GSs) and affect gluten functionality and end-use quality of common wheat, could be isolated simultaneously. Three deletion lines missing Glu-A1, Glu-B1 or Glu-D1 were developed from the original mutants, with the Glu-1 genomic regions deleted in these lines estimated using newly developed DNA markers. Apart from lacking the target HMW-GSs, the three lines all showed decreased accumulation of low molecular weight glutenin subunits (LMW-GSs) and increased amounts of gliadins. Based on the test data of five gluten and glutenin macropolymer (GMP) parameters obtained with grain samples harvested from two environments, we conclude that the genetic effects of Glu-1 loci on gluten functionality can be ranked as Glu-D1 > Glu-B1 > Glu-A1. Furthermore, it is suggested that Glu-1 loci contribute to gluten functionality both directly (by promoting the formation of GMP) and indirectly (through keeping the balance among HMW-GSs, LMW-GSs and gliadins). Finally, the efficient isolation of ion beam mutations for functional comparison of homoeologous loci in polyploid plants and the usefulness of Glu-1 deletion lines for further studying the contribution of Glu-1 loci to gluten functionality are discussed.     

Effect of 2,5-dibromo-3-methyl-6-isopropyl-p-benzoquinone on the secondary electron acceptor B of photosystem II

Measurements of chlorophyll fluorescence have been used to monitor electron transport from the primary electron acceptor of photosystem II, Q, to the secondary acceptor, B, in chloroplasts in either the presence or the absence of the plastoquinone analog 2,5-dibromo-3-methyl-6-isopropyl-p-benzoquinone (DBMIB). Electron transport is markedly slower from Q^? to either B or B^? in the presence of DBMIB. Binary oscillations in the rate of reoxidation of Q^? (equivalent to the reactions Q^?B → QB^? and Q^?B^? → QB^2?) after each of a series of flashes were of a phase opposite to those observed in the absence of DBMIB (J. M. Bowes, and A. R. Crofts, (1980) Biochim. Biophys. Acta590, 573–584). The results confirm that inhibition of electron transport by DBMIB in chloroplasts is not restricted to an inhibition of electron transfer from the plastoquinone pool, but that there is also a specific interaction between the reduced form of the inhibitor and the secondary electron acceptor B. Models are discussed to account for the mechanism of this interaction.     

A map of the Monte Arci (Sardinia Island, Western Mediterranean) obsidian primary to secondary sources. Implications for Neolithic provenance studies

Four types of obsidians from the Monte Arci volcanic complex (Sardinia) were used by Neolithic men in the North Tyrrhenian area of the western Mediterranean. A map of their occurrences from primary sources (mother rocks) to distant secondary deposits in the surrounding plains is presented. Some 1457 specimens were macroscopically characterized and in addition ~15% of them fingerprinted from their elemental compositions as determined by electron microprobe, neutron activation analysis or ion beam analysis. The results show that secondary sources, up to now largely neglected in provenance studies of ‘archaeological’ obsidians will have from now to be taken into account. To cite this article: C. Lugliè et al., C. R. Palevol 5 (2006).     

Synthesis, structures and luminescent properties of new heterobimetallic Zn-4f Schiff base complexes

A series of new 3d-4f heterobimetallic Schiff base complexes of the general formula [Zn(μ-L²)Ln(NO₃)₃(H₂O)_n] (Ln = La 1, Nd 2, Gd 3, Er 4 and Yb 5; n = 1 or 2; H₂L² = N,N′-bis(3-methoxy-5-p-tolylsalicylidene)ethylene-1,2-diamine) are synthesized and characterized. Complexes 1, 2, 4 and 5 are structurally characterized by X-ray crystallography. The photophysical properties of these complexes are also investigated. At room temperature, complexes 1-5 exhibit similar solution absorption and emission spectra in the UV-Vis region. Furthermore, compounds 2, 4 and 5 exhibit solution emission corresponding to the lanthanide(III) ion in the near-infrared region at room temperature. The triplet state emission of the 3d-4f bimetallic complexes without energy transfer is also determined through the photophysical study of complex 3.     

A computational approach to design energetic ionic liquids

The present work deals with the theoretical estimation of ion-pair binding energies and the energetic properties of four ion pairs formed by combining the 1-butyl-2,4-dinitro-3-methyl imidazolium ion with nitrate (I), perchlorate (II), dinitramide (III), or 3,5-dinitro-1,2,4-triazolate (IV) anions. The counterpoise-corrected ion-pair binding energies were calculated for each ion pair at the B3LYP/6-311+G(d,p) level of theory. Results show that the cation–anion interaction is strongest for ion pair I and weakest for IV, indicating that the nitrate (I) has a greater tendency to exist as a stable ionic salt whereas the 3,5-dinitro-1,2,4-triazolate (IV) may exist as an ionic liquid. Natural bond orbital (NBO) analysis and electrostatic potential (ESP) mapping revealed that charge transfer occurs in all of the ion pairs, but is greatest (0.25e) for ion pair I and smallest (0.03e) for IV, resulting in ion pair I being the least polarized. A nucleus-independent chemical shift (NICS) study revealed that the aromaticity of the 1-butyl-2,4-dinitro-3-methyl imidazolium ion significantly increases in ion pair IV, indicating that this has the greatest charge delocalization among all of the four ion pairs considered. Studies of thermodynamic and detonation properties showed that ion pair II is the most energetic ion pair in terms of its detonation velocity (D = 7.5 km s^?1) and detonation pressure (P = 23.1 GPa). It is also envisaged that ion pair IV would exist as an energetic azolium azolate type ionic liquid that could be conveniently used as a secondary explosive characterized by detonation parameters D and P of 6.9 km s^?1 and 19.3 GPa, respectively. These values are comparable to those of conventional explosives such as TNT.     

Effect of space charge on the energy spectrum of a multispecies ion beam

The parameters of a multispecies metal ion beam extracted with the help of a set of grids from a plasma jet of a pulsed vacuum arc are studied experimentally. It is shown that the beam contains ions with energies that are both significantly lower and higher than the expected energy E _Z = \(\bar Z\) eU _acc, where \(\bar Z\) is the average ion charge number and U _acc is the extracting voltage. As a result, the mean ion energy is lower than E _Z and the ion energy spectrum is substantially wider than that in the plasma jet. It is found that this effect weakens with decreasing discharge current amplitude and that the shape of the spectrum depends on the accelerating voltage. Probe measurements show that, at accelerating voltages higher than 1 kV, a positive space charge forms in the drift gap, due to which the electric potential in the drift gap increases to a few hundred electronvolts. Analysis of experimental data indicates that the observed features of the ion spectrum can be attributed to the effect of the unsteady electric field of the space charge of the ion beam transported through the drift gap.     

Ultrahigh charging of dust grains by the beam−plasma method for creating a compact neutron source

Generation of high-voltage high-current electron beams in a low-pressure (P = 0.1–1 Torr) gas discharge is studied experimentally as a function of the discharge voltage and the sort and pressure of the plasma-forming gas. The density of the plasma formed by a high-current electron beam is measured. Experiments on ultrahigh charging of targets exposed to a pulsed electron beam with an energy of up to 25 keV, an electron current density of higher than 1 A/cm², a pulse duration of up to 1 μs, and a repetition rate of up to 1 kHz are described. A numerical model of ultrahigh charging of dust grains exposed to a high-energy electron beam is developed. The formation of high-energy positive ions in the field of negatively charged plane and spherical targets is calculated. The calculations performed for a pulse-periodic mode demonstrate the possibility of achieving neutron yields of higher than 10⁶ s^–1 cm^–2 in the case of a plane target and about 10⁹ s^–1 in the case of 10³ spherical targets, each with a radius of 250 μm.