Investigation of nanopore evolution in ion track-etched polycarbonate membranes

Single heavy ion tracks in polycarbonate foils were chemically etched in an electrolytical cell under various conditions (different temperatures, etchant concentrations, and applied potentials), and the pore evolution was monitored by measuring the current through the membrane. Different zones of the latent tracks could be identified via changes in the radial etching rate with time. Further it was found that the shape of the radial etching rate versus time curves depends on temperature, etchant concentration, and applied voltage. The functionalities are attributed to etching products (double-charged diphenylol-propane anions), which are adsorbed on the pore walls and, thus, affect the further etching process.     

Preparation, sintering and leaching of optimized uranium thorium dioxides

Mixed actinide dioxides are currently studied as potential fuels for several concepts associated to the fourth generation of nuclear reactors. These solids are generally obtained through dry chemistry processes from powder mixtures but could present some heterogeneity in the distribution of the cations in the solid. In this context, wet chemistry methods were set up for the preparation of U_1−xTh_xO₂ solid solutions as model compounds for advanced dioxide fuels. Two chemical routes of preparation, involving the precipitation of crystallized precursor, were investigated: on the one hand, a mixture of acidic solutions containing cations and oxalic acid was introduced in an open vessel, leading to a poorly-crystallized precipitate. On the other hand, the starting mixture was placed in an acid digestion bomb then set in an oven in order to reach hydrothermal conditions. By this way, small single-crystals were obtained then characterized by several techniques including XRD and SEM. The great differences in terms of morphology and crystallization state of the samples were correlated to an important variation of the specific surface area of the oxides prepared after heating, then the microstructure of the sintered pellets prepared at high temperature. Preliminary leaching tests were finally undertaken in dynamic conditions (i.e. with high renewal of the leachate) in order to evaluate the influence of the sample morphology on the chemical durability of the final cohesive materials.     

Applications of MeV ion beams to material processing

The development of commercial ion implanters capable of implanting a wide range of elements with multi MeV energies has enabled ion implantation to be applied effectively to the modification of materials to a depth of several micrometers. For a silicon semiconductor technology the depth of penetration enables buried layers to be placed behind device structures to act as electrically isolating barriers. For high mass binary or ternary semiconductors, MeV ion implantation may be the only method of doping without resorting to chemically less pure film deposition techniques which tend to be unsuitable for large scale integration. In metals relatively thick (~1 μm) coatings can be penetrated to improve adhesion. Also, the corrosion properties of metals may be altered by changing the oxidation properties or by the creation of thick amorphous alloy coatings. With these effects come the added advantages that the smoothness and continuity of the surface is retained or may be enhanced. For polymers, MeV implantation enables thick electronic, wear or chemical modifications to be made to the material without loss of bulk integrity or properties.     

Comparison of secondary electron emission in helium ion microscope with gallium ion and electron microscopes

To evaluate secondary electron (SE) image characteristics in helium ion microscope, Si surfaces with a rod and step structures is scanned by 30 keV He and Ga ion beams and 1 keV electron beam. The topographic sensitivity of He ions is in principle higher than that for scanning electron microscope (SEM) because of the stronger dependency of SE yield versus incident angle for He ions. As shrinking to sub nm patterns, the pseudo-images constructed from line profile of SE intensity by the electron beam lose their sharpness, however, the images for the He and Ga ion beams keep clearness due to darkening the bottom corners of the pattern. Here, the sputter erosion for Ga ions must be considered. Furthermore, trajectories of emitted SEs are simulated for a rectangular Al surface scanned by the beams to study voltage contrast, where positive and negative voltages are applied to the small area of the sample. Both less high energy component in the energy distribution of SEs and dominant contribution of direct SE excitation by a projectile He ion keep a high voltage contrast down to a sub nm sized area positively biased against the zero-potential surroundings.     

Real-time X-ray studies of the growth of Mo-seeded Si nanodots by low-energy ion bombardment

Silicon surface evolution during room temperature low-energy (300, 500 and 1000 eV) normal incidence Ar⁺ ion bombardment in the presence of Mo seed atoms has been studied with real-time grazing-incidence small-angle X-ray scattering and ex situ atomic force microscopy. When a small amount of Mo atoms was supplied to the Si surface during ion bombardment, the development of correlated structures with two different characteristic length scales was observed. The shorter length scale features (“dots”) coarsened with time until they reached a constant spatial wavelength. The longer length scale corrugations associated with kinetic roughening, however, continued to grow in amplitude during bombardment. The overall roughness is dominated by different corrugations at different times in the kinetic evolution, showing a complex behavior. The evolution of the kinetic roughening can be described by the Family-Vicsek scaling hypothesis, but measured scaling exponents are not in agreement with those of existing models.     

离子束电子束多功能材料表面处理设备

本设备由以下系统组成:注入系统,有溅射离子源及不对称三电极加速管,能量50keV,流强4mA(N~+);电子束系统,能量45keV,功率密度10~2—10~6W/ cm~2;配备微机程序的束偏摆装置;靶材易换的磁控溅射靶;可作旋转、平移、升降等机械运动的高真空工作室(φ500×1600mm)。可进行离子注入及混合、电子束上釉及合金化、磁控溅射离子镀等工艺。该设备为材料表面改性和薄膜制备提供了新的手段。     

The optimization of gamma spectra processing in prompt gamma neutron activation analysis (PGNAA)

The uncertainty of the elemental analysis is one of the major factors governing the utility of on-line Prompt Gamma Neutron Activation Analysis (PGNAA) in the blending and sorting of bulk materials. In this paper, a general method applicable to Gamma spectra processing is presented and applied to PGNAA in mineral industry. Based on the Fourier transform of spectra and their de-correlation in the Fourier space (the improvement of the conditioning of the correlation matrix), processing of overlapping of characteristic peaks minimizes the propagation of random errors, which optimizes the accuracy and decreases the detection limits of elemental analyses. In comparison with classical methods based on the linear combinations of relevant regions of spectra the improvement may be considerable, especially when several elements are interfering. The method is applied to four case stories covering both borehole logging and on-line analysis on conveyor belt of raw materials.     

Correlation between ion beam parameters and physical characteristics of nanostructures fabricated by focused ion beam

We report a study of the physical characteristics of the pillars of C, Pt and W grown by 10-30 keV Ga focused ion beam (FIB) as a function of Ga ion flux, and present a quantitative analysis of the elements using energy-dispersive analysis of X-rays (EDAX). All the FIB grown pillars exhibit a rough morphology with whisker like protrusions on the cylindrical surface and broadening of the base as compared to the nominal size. For a constant fluence, the height of the pillar initially increases and then reduces after going through a maximum as a function of ion flux in all the cases. The compositional analysis shows good metallic quality for Pt structures but reveals significant contamination of Ga in C and Ga and C in W structures at higher ion fluxes. Explanation to all these observations has been sought in the light of secondary ion and electron effects and the different processes involved which lead to the FIB induced deposition.     

Accurate location and marking of grain boundaries using focused ion and electron beams

We have investigated the 2×12° symmetric grain boundary of (0 0 1) oriented bicrystalline silicon substrates for high-T_c superconductor applications using scanning focused ion beam (FIB) and electron beam (SEM). We successfully used the focused ion beam to detect and to mark the grain boundary and hence, to increase the accuracy of positioning the Josephson device with respect to the grain boundary of the silicon substrate. Both imaging methods have been compared using channeling effects of focused ion and electron beams in a dual beam system.     

Amorphous phase and anisotropy induced by glancing incident ion beams in Co-Nb films

Co-Nb amorphous films were prepared with the aid of glancing incident ion beams during deposition process. Influence of ion interaction to phase formation and fine microstructure was studied. Amorphous range is about 19 to 63 at.% Co fractions, which is wider than that obtained by perpendicular ion bombardment (28 to 68 at.% of Co fractions). A ripple or a bamboo raft pattern with nano-scale periodicity is observed in the TEM (transmission electron microscopy), SEM (scanning electron microscopy) and AFM (atomic force microscopy) images. The sizes of the image patterns are characterized by correlation length calculated from height-height correlation function (HHCF). The correlation length along the ion incidence is longer than that perpendicular to the ion incidence. Analysis regards that the glancing incident ion beams have high efficiency in both rapid cooling and ion mixing (IM). The main pattern feature in the images mainly comes from surface erosion. Other fine microstructure and the difference among the images result from surface diffusion or viscous flow effect.     

Creation mechanism of pores by ion beam modification of fluoropolymer film membranes

Producing structures in membranes at the nanometer scale can serve several applications such as to localize molecular electrical junctions and switches, and to function as masks. In previous work we demonstrated the fabrication of porous membranes in masked fluoropolymer films using scanned ion beam bombardment. The process dispenses the use of time consuming chemical and etching processes. Here we report on the creation mechanism of pores using ion bombardment. Aspects of the ion beam interaction with matter are explained as well as an analysis of the shape of the fabricated structures. The pores were produced using our feedback controlled ion beam apparatus and were analyzed using optical and atomic force microscopic (AFM) analyses.     

Field structure and electron life times in the MEFISTO electron cyclotron resonance ion source

The complex magnetic field of the permanent magnet electron cyclotron resonance (ECR) ion source MEFISTO located at the University of Berne has been numerically simulated. For the first time the magnetized volume qualified for electron cyclotron resonance at 2.45 GHz and 87.5 mT has been analyzed in highly detailed 3D simulations with unprecedented resolution. New results were obtained from the numerical simulation of 25,211 electron trajectories. The evident characteristic ion sputtering trident of hexapole confined ECR ion sources has been identified with the field and electron trajectory distribution. Furthermore, unexpected long electron trajectory lifetimes were found.     

Production of intense highly charged ion beams by IMP 14.5 GHz electron cyclotron resonance ion source

A new 14.5GHz Electron Cyclotron Resonance(ECR) ion source has been constructed over the last two years.The source was designed and tested by making use of the latest results from ECR ion source development ,such as high mirror magnetic filed,large plasma volume,and biased probe.140μA of O^7 ,185μA of Ar^11 and 50 μA of Xe^26 could be produced with a RF power of 800W, The intense beams of highly charged metallic ions are produced by means of the method of a metal evaporation oven and volatile compound throuth axial access,The test results are 130μA of Ca^11 ,70μA of Ca^12 and 65 μA of Fe^10 ,The ion source has been put into operation for the cyclotron at the Institute of Moderm Physics(IMP).     

Performance of the SIRAD ion electron emission microscope

An axial ion electron emission microscope (IEEM) is now working at the SIRAD irradiation facility of the INFN Laboratories of Legnaro (Italy). The IEEM is used to precisely reconstruct the impact points of single ions, information that may be used to determine the areas of a microelectronic device under test that are sensitive to single event effects (SEE). After describing the setup briefly reviewing its working principles, we show our first time resolved ion induced electron emission images of standard calibration targets. We also discuss a preliminary measurement of ion impact detection efficiency of the IEEM system and the available trigger signals for SEE studies. We finally make an assessment of ion electron emission microscopy at SIRAD and indicate future developments.     

离子束—电子束—原子束结合沉积技术制成膜的形貌特征

简要介绍离子束-电子束-原子束结合沉积技术的原理及特点,并对该技术制备的各种合金、陶瓷以及复合膜的形貌特征进行了分析研究。     

电子回旋共振离子源的研制及应用

描述了一台电子回旋共振离子源的设计,结构及特性。及了获得离子源的长寿命,较高的等离子密度以及高效的传输微波功率,利用合适的三层微波输入窗是很有效。采用两个带有磁轭的螺线管线圈能够产生满足共振条件和约束等离子的轴向磁场。     

Cross-section transmission electron microscopy of the ion implantation damage in annealed diamond

It has formerly been shown that low-damage levels, produced during the implantation doping of diamond as a semiconductor, anneal easily while high levels “graphitize” (above about 5.2 × 10¹⁵ ions/cm²). The difference in the defect types and their profiles, in the two cases, has never been directly observed. We have succeeded in using cross-section transmission electron microscopy to do so. The experiments were difficult because the specimens must be polished to ∼40 μm thickness, then implanted on edge and annealed, before final ion beam thinning to electron transparency. The low-damage micrographs reveal some deeply penetrating dislocations, whose existence had been predicted in earlier work.     

Recent progress in emulsion technology to study fragmentation reactions of high energetic ion beams

The R&D project to study nuclear fragmentation using emulsion in attempt to improve the accuracy of dose calculation in carbon ion radiotherapy has been carried out at NIRS-HIMAC since 2003. Based on the developed techniques, we are accumulating experimental data of fragmentation reactions for various beams and target combinations. In this program we are also developing the practical application of hybrid apparatus of emulsion and CR-39 and performing basic study of gold deposition development in order to improve measurement of ionization.     

Deposition of zirconium carbonitride composite films using ion and electron beams emitted from plasma focus device

Nanocrystalline zirconium carbonitride (ZrCN) composite films were deposited on zirconium substrates for multiple (10, 20, 30, 40 and 50) focus shots. X-ray diffraction analysis shows diffraction peaks corresponding to nitrides (ZrN, Zr₂N and Zr₃N₄), carbide (ZrC) and carbonitride (Zr₂CN), confirming the formation of ZrCN composite films. The average crystallite size estimated for ZrN (2 0 0) and Zr₂CN (1 1 1) planes are found to vary from 10 to 20 nm. Maximum compressive stresses of ∼3.9 GPa in Zr₂N (0 0 2) plane for 30 focus shots and maximum tensile stresses of ∼6.5 GPa in ZrN (2 0 0) plane for 20 focus shots are observed. Tensile stresses observed in Zr₂CN (1 1 1) plane are transformed to compressive stresses for higher (40 and 50) focus shots. Raman analysis reveals the emergence of D and G bands related to carbide phases during the film deposition process. Scanning electron microscope analysis exhibits the nanocrystalline microstructure patterns of the composite films. Microstructure patterns showing agglomerates of 30-300 nm dimensions are also observed. Microhardness values of ZrCN composite films increases with increasing number of focus shots and is equal to 5.6 ± 0.45 GPa for 10 g imposed load, which is 4.5 times that of the virgin one.